Electronic Supplementary MAterial for CrystEngComm This Journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Ian Dance' 'Hong Chow' 'Don Craig' 'Felicia Maharaj' 'Michael Page' 'Vanessa Russell' 'Marcia L. Scudder' _publ_contact_author_name 'Prof Ian Dance' _publ_contact_author_address ; School of Chemical Sciences University of New South Wales UNSW Sydney NSW 2052 AUSTRALIA ; _publ_contact_author_email I.DANCE@UNSW.EDU.AU _publ_section_title ; Polymorphs and pseudo-polymorphs: nine crystals containing [Fe(phen)3]2+ associated with [HgI4]2-. ; _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. De Meulenaer, J. and Tompa, H. Acta Cryst., 1965, 19, 1014. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1989. ; data_DID260_F-(ethanol)(CH3CN) _database_code_CSD 212709 _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C36 H24 Fe N6 2+,Hg I4 2-,C2 H3 N,C2 H6 O' _chemical_formula_sum 'C40 H33 Fe Hg I4 N7 O' _chemical_formula_iupac ? _chemical_formula_weight 1391.8 # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2-y,-z 3 -x,1/2+y,1/2-z 4 1/2-x,-y,1/2+z 5 -x,-y,-z 6 1/2-x,1/2+y,z 7 x,1/2-y,1/2+z 8 1/2+x,y,1/2-z _cell_length_a 16.248(4) _cell_length_b 19.603(4) _cell_length_c 26.440(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8421(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12 _cell_measurement_temperature 294 _exptl_crystal_description multifacetted _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.20 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5184.0 _exptl_absorpt_coefficient_mu 6.927 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.31 _exptl_absorpt_correction_T_max 0.43 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 5823 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 23 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 4 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 5823 _reflns_number_gt 3236 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_ref 0.047 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3236 _refine_ls_number_parameters 271 _refine_ls_goodness_of_fit_ref 1.34 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.007 _refine_diff_density_max 1.67 _refine_diff_density_min -1.81 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Fe 0.28335(10) 0.35613(9) 0.37857(6) 0.0345(5) Uani Fe 1.0 N1A 0.3958(6) 0.3950(5) 0.3796(3) 0.037(2) Uani N 1.0 N2A 0.2616(7) 0.4277(5) 0.4292(4) 0.039(2) Uani N 1.0 C1A 0.4640(8) 0.3750(7) 0.3576(5) 0.045(2) Uani C 1.0 C2A 0.5392(8) 0.4067(8) 0.3632(5) 0.055(2) Uani C 1.0 C3A 0.5437(9) 0.4636(8) 0.3937(5) 0.056(2) Uani C 1.0 C4A 0.4738(9) 0.4861(7) 0.4178(5) 0.049(2) Uani C 1.0 C5A 0.4742(10) 0.5451(7) 0.4505(6) 0.061(3) Uani C 1.0 C6A 0.4045(11) 0.5624(7) 0.4746(6) 0.064(4) Uani C 1.0 C7A 0.3281(10) 0.5250(7) 0.4700(5) 0.056(3) Uani C 1.0 C8A 0.2551(11) 0.5367(8) 0.4980(5) 0.069(4) Uani C 1.0 C9A 0.1897(10) 0.4936(8) 0.4897(5) 0.065(3) Uani C 1.0 C10A 0.1926(9) 0.4420(7) 0.4538(5) 0.049(2) Uani C 1.0 C11A 0.3288(9) 0.4688(7) 0.4374(5) 0.043(2) Uani C 1.0 C12A 0.4012(9) 0.4502(7) 0.4112(4) 0.040(2) Uani C 1.0 N1B 0.2424(6) 0.4155(5) 0.3234(4) 0.037(2) Uani N 1.0 N2B 0.1683(6) 0.3246(5) 0.3776(4) 0.038(2) Uani N 1.0 C1B 0.2832(9) 0.4610(7) 0.2948(5) 0.045(2) Uani C 1.0 C2B 0.2454(9) 0.4982(7) 0.2558(5) 0.056(2) Uani C 1.0 C3B 0.1641(9) 0.4895(8) 0.2458(5) 0.056(2) Uani C 1.0 C4B 0.1196(9) 0.4415(7) 0.2747(5) 0.047(2) Uani C 1.0 C5B 0.0342(9) 0.4267(8) 0.2695(5) 0.054(3) Uani C 1.0 C6B -0.0063(8) 0.3803(8) 0.2967(5) 0.055(3) Uani C 1.0 C7B 0.0384(8) 0.3416(8) 0.3353(5) 0.049(2) Uani C 1.0 C8B 0.0010(8) 0.2924(8) 0.3648(5) 0.060(3) Uani C 1.0 C9B 0.0478(9) 0.2605(8) 0.4005(6) 0.059(3) Uani C 1.0 C10B 0.1309(8) 0.2783(7) 0.4066(5) 0.047(2) Uani C 1.0 C11B 0.1207(8) 0.3559(7) 0.3435(5) 0.040(2) Uani C 1.0 C12B 0.1620(8) 0.4063(7) 0.3126(5) 0.040(2) Uani C 1.0 N1C 0.3141(6) 0.2831(5) 0.3314(4) 0.037(2) Uani N 1.0 N2C 0.3182(6) 0.2889(5) 0.4297(4) 0.036(2) Uani N 1.0 C1C 0.3110(8) 0.2815(7) 0.2798(5) 0.043(2) Uani C 1.0 C2C 0.3391(9) 0.2260(8) 0.2524(5) 0.052(3) Uani C 1.0 C3C 0.3697(9) 0.1709(8) 0.2763(5) 0.054(3) Uani C 1.0 C4C 0.3718(8) 0.1685(7) 0.3285(5) 0.047(2) Uani C 1.0 C5C 0.3998(8) 0.1115(7) 0.3577(5) 0.054(2) Uani C 1.0 C6C 0.4027(8) 0.1139(7) 0.4090(5) 0.053(3) Uani C 1.0 C7C 0.3759(8) 0.1746(7) 0.4360(5) 0.045(2) Uani C 1.0 C8C 0.3791(8) 0.1799(8) 0.4891(5) 0.051(3) Uani C 1.0 C9C 0.3524(9) 0.2403(8) 0.5107(5) 0.049(3) Uani C 1.0 C10C 0.3215(8) 0.2928(7) 0.4793(5) 0.041(2) Uani C 1.0 C11C 0.3460(8) 0.2288(7) 0.4073(5) 0.038(2) Uani C 1.0 C12C 0.3441(8) 0.2260(7) 0.3547(5) 0.039(2) Uani C 1.0 Hg 0.69505(3) 0.23731(3) 0.37238(2) 0.0470(2) Uani Hg 1.0 I1 0.77464(5) 0.36388(5) 0.36451(4) 0.0505(3) Uani I 1.0 I2 0.81344(6) 0.13269(5) 0.37693(4) 0.0586(3) Uani I 1.0 I3 0.59813(7) 0.23138(7) 0.28640(4) 0.0709(4) Uani I 1.0 I4 0.59627(7) 0.23582(7) 0.45642(4) 0.0799(4) Uani I 1.0 N1An 0.4885(10) 0.0421(8) 0.5735(6) 0.085(5) Uani N 1.0 C1An 0.4458(11) 0.0088(10) 0.5987(8) 0.072(6) Uani C 1.0 C2An 0.3940(11) -0.0343(9) 0.6300(8) 0.104(7) Uani C 1.0 O1Et 0.5579(11) 0.0734(8) 0.2271(8) 0.178(9) Uani O 1.0 C1Et 0.5663(17) 0.1013(12) 0.1846(8) 0.112(8) Uani C 1.0 C2Et 0.6475(14) 0.1220(11) 0.1617(7) 0.113(8) Uani C 1.0 HC1A 0.4612 0.3339 0.3351 0.049 Uani H 1.0 HC2A 0.5893 0.3888 0.3457 0.067 Uani H 1.0 HC3A 0.5971 0.4882 0.3982 0.067 Uani H 1.0 HC5A 0.5255 0.5727 0.4551 0.071 Uani H 1.0 HC6A 0.4054 0.6034 0.4971 0.079 Uani H 1.0 HC8A 0.2513 0.5749 0.5230 0.086 Uani H 1.0 HC9A 0.1385 0.4997 0.5101 0.080 Uani H 1.0 HC10A 0.1417 0.4151 0.4464 0.051 Uani H 1.0 HC1B 0.3430 0.4686 0.3015 0.049 Uani H 1.0 HC2B 0.2784 0.5313 0.2354 0.068 Uani H 1.0 HC3B 0.1365 0.5165 0.2186 0.065 Uani H 1.0 HC5B 0.0024 0.4529 0.2435 0.062 Uani H 1.0 HC6B -0.0663 0.3721 0.2909 0.065 Uani H 1.0 HC8B -0.0584 0.2806 0.3601 0.072 Uani H 1.0 HC9B 0.0229 0.2244 0.4224 0.072 Uani H 1.0 HC10B 0.1635 0.2552 0.4337 0.049 Uani H 1.0 HC1C 0.2879 0.3217 0.2613 0.044 Uani H 1.0 HC2C 0.3365 0.2268 0.2146 0.062 Uani H 1.0 HC3C 0.3911 0.1315 0.2562 0.064 Uani H 1.0 HC5C 0.4175 0.0690 0.3398 0.063 Uani H 1.0 HC6C 0.4233 0.0736 0.4283 0.060 Uani H 1.0 HC8C 0.3999 0.1414 0.5104 0.059 Uani H 1.0 HC9C 0.3549 0.2467 0.5481 0.058 Uani H 1.0 HC10C 0.3010 0.3355 0.4958 0.043 Uani H 1.0 H1C1Et 0.5329 0.1441 0.1862 0.112 Uani H 1.0 H2C1Et 0.5409 0.0691 0.1598 0.112 Uani H 1.0 H1C2Et 0.6378 0.1430 0.1278 0.113 Uani H 1.0 H2C2Et 0.6753 0.1558 0.1843 0.113 Uani H 1.0 H3C2Et 0.6833 0.0808 0.1578 0.113 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Fe 0.036(1) 0.040(1) 0.027(1) 0.0052(9) 0.0012(8) -0.0004(9) Fe N1A 0.048(3) 0.039(3) 0.024(3) 0.014(2) -0.002(2) 0.004(2) N N2A 0.055(3) 0.037(3) 0.025(3) 0.018(2) -0.001(2) -0.004(2) N C1A 0.047(3) 0.054(3) 0.032(3) 0.014(2) 0.001(2) 0.004(2) C C2A 0.049(3) 0.072(6) 0.044(5) 0.008(3) -0.001(2) 0.011(3) C C3A 0.056(3) 0.066(5) 0.046(6) -0.002(3) -0.011(3) 0.016(3) C C4A 0.063(3) 0.047(3) 0.038(4) 0.001(3) -0.014(3) 0.009(2) C C5A 0.085(4) 0.047(4) 0.050(5) -0.004(4) -0.025(4) 0.005(3) C C6A 0.097(6) 0.043(4) 0.052(5) 0.005(4) -0.023(4) -0.009(3) C C7A 0.084(4) 0.043(3) 0.043(3) 0.016(3) -0.012(3) -0.013(3) C C8A 0.096(6) 0.059(4) 0.052(4) 0.025(4) -0.004(4) -0.028(4) C C9A 0.081(4) 0.068(5) 0.047(4) 0.029(4) 0.005(4) -0.025(4) C C10A 0.061(3) 0.053(3) 0.034(3) 0.023(3) 0.004(3) -0.011(2) C C11A 0.063(3) 0.036(3) 0.030(3) 0.015(2) -0.007(2) -0.004(2) C C12A 0.056(3) 0.037(3) 0.028(3) 0.010(2) -0.008(2) 0.004(2) C N1B 0.045(2) 0.039(3) 0.028(3) 0.010(2) 0.006(2) -0.001(2) N N2B 0.040(3) 0.044(3) 0.030(3) 0.006(2) 0.008(2) -0.003(2) N C1B 0.056(3) 0.045(4) 0.034(3) 0.006(2) 0.005(2) 0.006(2) C C2B 0.072(4) 0.054(4) 0.041(3) 0.007(4) 0.000(3) 0.013(3) C C3B 0.072(4) 0.055(5) 0.039(3) 0.018(4) -0.004(3) 0.007(3) C C4B 0.055(3) 0.052(4) 0.034(3) 0.020(3) -0.001(2) -0.003(2) C C5B 0.053(3) 0.068(6) 0.040(4) 0.024(3) -0.004(3) -0.010(3) C C6B 0.045(2) 0.078(6) 0.044(5) 0.018(3) -0.002(3) -0.013(3) C C7B 0.041(3) 0.068(4) 0.041(3) 0.008(2) 0.004(2) -0.009(2) C C8B 0.043(3) 0.085(6) 0.052(5) -0.005(3) 0.006(2) -0.004(4) C C9B 0.049(3) 0.078(5) 0.052(5) -0.011(3) 0.008(3) 0.004(3) C C10B 0.046(2) 0.056(4) 0.039(3) -0.002(3) 0.008(2) 0.002(2) C C11B 0.040(3) 0.049(3) 0.032(2) 0.010(2) 0.006(2) -0.006(2) C C12B 0.045(2) 0.044(3) 0.030(3) 0.014(2) 0.004(2) -0.004(2) C N1C 0.034(3) 0.045(2) 0.030(2) 0.000(2) 0.002(2) -0.003(2) N N2C 0.032(3) 0.046(2) 0.030(2) 0.000(2) 0.001(2) 0.002(2) N C1C 0.046(3) 0.053(3) 0.030(2) 0.002(2) 0.002(3) -0.006(2) C C2C 0.061(6) 0.060(4) 0.037(2) 0.006(4) 0.004(3) -0.012(3) C C3C 0.062(5) 0.055(3) 0.046(3) 0.008(3) 0.007(4) -0.013(3) C C4C 0.049(3) 0.047(2) 0.047(3) 0.005(2) 0.005(3) -0.006(2) C C5C 0.054(4) 0.047(3) 0.060(4) 0.008(2) 0.007(4) -0.002(2) C C6C 0.050(4) 0.047(3) 0.060(4) 0.008(3) 0.004(4) 0.006(3) C C7C 0.042(3) 0.049(2) 0.046(3) 0.005(2) 0.002(3) 0.007(2) C C8C 0.050(5) 0.058(3) 0.045(2) 0.007(3) 0.000(4) 0.014(3) C C9C 0.051(5) 0.062(4) 0.035(2) 0.006(4) -0.002(3) 0.010(3) C C10C 0.041(3) 0.054(3) 0.030(2) 0.002(2) 0.000(3) 0.004(2) C C11C 0.034(3) 0.045(2) 0.036(2) 0.002(2) 0.002(2) 0.002(2) C C12C 0.037(3) 0.044(2) 0.037(2) 0.002(2) 0.003(2) -0.002(2) C Hg 0.0476(3) 0.0515(4) 0.0417(3) -0.0008(3) 0.0010(3) -0.0006(3) Hg I1 0.0445(5) 0.0473(6) 0.0598(6) -0.0037(5) 0.0022(5) 0.0002(5) I I2 0.0705(7) 0.0486(6) 0.0566(6) 0.0144(6) 0.0004(5) 0.0017(6) I I3 0.0652(8) 0.0941(9) 0.0534(7) 0.0005(7) -0.0172(6) -0.0129(7) I I4 0.0681(9) 0.124(1) 0.0473(7) -0.0170(8) 0.0168(6) -0.0065(7) I N1An 0.087(9) 0.083(9) 0.085(9) 0.011(9) -0.002(9) -0.006(9) N C1An 0.059(9) 0.067(9) 0.091(9) 0.025(9) -0.026(9) -0.025(9) C C2An 0.079(9) 0.064(9) 0.168(9) -0.007(9) 0.021(9) 0.028(9) C O1Et 0.196(9) 0.091(9) 0.247(9) 0.025(9) 0.128(9) 0.050(9) O C1Et 0.177(9) 0.093(9) 0.066(9) -0.038(9) -0.001(9) -0.026(9) C C2Et 0.153(9) 0.095(9) 0.090(9) -0.007(9) 0.021(9) 0.032(9) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1A 1.981(10) 1_555 1_555 no Fe N2A 1.972(10) 1_555 1_555 no Fe N1B 1.982(10) 1_555 1_555 no Fe N2B 1.969(10) 1_555 1_555 no Fe N1C 1.962(10) 1_555 1_555 no Fe N2C 1.972(10) 1_555 1_555 no N1A C1A 1.312(14) 1_555 1_555 no N1A C12A 1.369(15) 1_555 1_555 no N2A C10A 1.326(15) 1_555 1_555 no N2A C11A 1.374(16) 1_555 1_555 no C1A C2A 1.380(18) 1_555 1_555 no C2A C3A 1.379(20) 1_555 1_555 no C3A C4A 1.375(19) 1_555 1_555 no C4A C5A 1.443(19) 1_555 1_555 no C4A C12A 1.385(18) 1_555 1_555 no C5A C6A 1.343(21) 1_555 1_555 no C6A C7A 1.446(20) 1_555 1_555 no C7A C8A 1.418(20) 1_555 1_555 no C7A C11A 1.398(17) 1_555 1_555 no C8A C9A 1.374(21) 1_555 1_555 no C9A C10A 1.388(17) 1_555 1_555 no C11A C12A 1.414(17) 1_555 1_555 no N1B C1B 1.343(15) 1_555 1_555 no N1B C12B 1.350(15) 1_555 1_555 no N2B C10B 1.334(15) 1_555 1_555 no N2B C11B 1.337(14) 1_555 1_555 no C1B C2B 1.404(17) 1_555 1_555 no C2B C3B 1.357(18) 1_555 1_555 no C3B C4B 1.412(19) 1_555 1_555 no C4B C5B 1.425(18) 1_555 1_555 no C4B C12B 1.398(17) 1_555 1_555 no C5B C6B 1.333(19) 1_555 1_555 no C6B C7B 1.465(18) 1_555 1_555 no C7B C8B 1.380(18) 1_555 1_555 no C7B C11B 1.384(17) 1_555 1_555 no C8B C9B 1.365(19) 1_555 1_555 no C9B C10B 1.404(18) 1_555 1_555 no C11B C12B 1.446(17) 1_555 1_555 no N1C C1C 1.365(14) 1_555 1_555 no N1C C12C 1.369(15) 1_555 1_555 no N2C C10C 1.313(14) 1_555 1_555 no N2C C11C 1.395(16) 1_555 1_555 no C1C C2C 1.386(17) 1_555 1_555 no C2C C3C 1.347(18) 1_555 1_555 no C3C C4C 1.381(17) 1_555 1_555 no C4C C5C 1.432(18) 1_555 1_555 no C4C C12C 1.397(17) 1_555 1_555 no C5C C6C 1.359(18) 1_555 1_555 no C6C C7C 1.454(18) 1_555 1_555 no C7C C8C 1.409(17) 1_555 1_555 no C7C C11C 1.392(17) 1_555 1_555 no C8C C9C 1.384(18) 1_555 1_555 no C9C C10C 1.415(17) 1_555 1_555 no C11C C12C 1.392(17) 1_555 1_555 no Hg I1 2.806(1) 1_555 1_555 no Hg I2 2.814(1) 1_555 1_555 no Hg I3 2.768(1) 1_555 1_555 no Hg I4 2.741(1) 1_555 1_555 no N1An C1An 1.162(21) 1_555 1_555 no C1An C2An 1.451(25) 1_555 1_555 no O1Et C1Et 1.258(22) 1_555 1_555 no C1Et C2Et 1.507(28) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Fe N2A 83.2(4) 1_555 1_555 1_555 no N1A Fe N1B 95.3(4) 1_555 1_555 1_555 no N1A Fe N2B 175.6(4) 1_555 1_555 1_555 no N1A Fe N1C 93.2(4) 1_555 1_555 1_555 no N1A Fe N2C 89.0(4) 1_555 1_555 1_555 no N2A Fe N1B 91.3(4) 1_555 1_555 1_555 no N2A Fe N2B 93.5(4) 1_555 1_555 1_555 no N2A Fe N1C 174.9(4) 1_555 1_555 1_555 no N2A Fe N2C 93.5(4) 1_555 1_555 1_555 no N1B Fe N2B 81.8(4) 1_555 1_555 1_555 no N1B Fe N1C 92.6(4) 1_555 1_555 1_555 no N1B Fe N2C 173.9(4) 1_555 1_555 1_555 no N2B Fe N1C 90.3(4) 1_555 1_555 1_555 no N2B Fe N2C 94.1(4) 1_555 1_555 1_555 no N1C Fe N2C 82.8(4) 1_555 1_555 1_555 no Fe N1A C1A 131.1(9) 1_555 1_555 1_555 no Fe N1A C12A 111.8(8) 1_555 1_555 1_555 no C1A N1A C12A 117.0(11) 1_555 1_555 1_555 no Fe N2A C10A 129.5(10) 1_555 1_555 1_555 no Fe N2A C11A 112.4(8) 1_555 1_555 1_555 no C10A N2A C11A 118.1(11) 1_555 1_555 1_555 no N1A C1A C2A 124.4(13) 1_555 1_555 1_555 no C1A C2A C3A 118.4(13) 1_555 1_555 1_555 no C2A C3A C4A 119.2(14) 1_555 1_555 1_555 no C3A C4A C5A 122.1(15) 1_555 1_555 1_555 no C3A C4A C12A 118.8(14) 1_555 1_555 1_555 no C5A C4A C12A 119.1(14) 1_555 1_555 1_555 no C4A C5A C6A 118.8(15) 1_555 1_555 1_555 no C5A C6A C7A 123.8(14) 1_555 1_555 1_555 no C6A C7A C8A 126.3(14) 1_555 1_555 1_555 no C6A C7A C11A 116.4(14) 1_555 1_555 1_555 no C8A C7A C11A 117.1(15) 1_555 1_555 1_555 no C7A C8A C9A 117.6(13) 1_555 1_555 1_555 no C8A C9A C10A 122.1(14) 1_555 1_555 1_555 no N2A C10A C9A 121.2(14) 1_555 1_555 1_555 no N2A C11A C7A 123.6(13) 1_555 1_555 1_555 no N2A C11A C12A 115.7(11) 1_555 1_555 1_555 no C7A C11A C12A 120.8(14) 1_555 1_555 1_555 no N1A C12A C4A 122.2(13) 1_555 1_555 1_555 no N1A C12A C11A 116.7(12) 1_555 1_555 1_555 no C4A C12A C11A 121.1(13) 1_555 1_555 1_555 no Fe N1B C1B 129.7(9) 1_555 1_555 1_555 no Fe N1B C12B 113.7(9) 1_555 1_555 1_555 no C1B N1B C12B 116.6(11) 1_555 1_555 1_555 no Fe N2B C10B 129.6(9) 1_555 1_555 1_555 no Fe N2B C11B 114.4(9) 1_555 1_555 1_555 no C10B N2B C11B 115.9(11) 1_555 1_555 1_555 no N1B C1B C2B 122.8(13) 1_555 1_555 1_555 no C1B C2B C3B 120.2(14) 1_555 1_555 1_555 no C2B C3B C4B 118.5(13) 1_555 1_555 1_555 no C3B C4B C5B 125.6(13) 1_555 1_555 1_555 no C3B C4B C12B 117.7(13) 1_555 1_555 1_555 no C5B C4B C12B 116.7(14) 1_555 1_555 1_555 no C4B C5B C6B 124.5(14) 1_555 1_555 1_555 no C5B C6B C7B 119.1(13) 1_555 1_555 1_555 no C6B C7B C8B 122.5(13) 1_555 1_555 1_555 no C6B C7B C11B 118.9(14) 1_555 1_555 1_555 no C8B C7B C11B 118.6(13) 1_555 1_555 1_555 no C7B C8B C9B 117.7(13) 1_555 1_555 1_555 no C8B C9B C10B 120.1(14) 1_555 1_555 1_555 no N2B C10B C9B 122.7(13) 1_555 1_555 1_555 no N2B C11B C7B 124.8(13) 1_555 1_555 1_555 no N2B C11B C12B 115.3(12) 1_555 1_555 1_555 no C7B C11B C12B 119.9(13) 1_555 1_555 1_555 no N1B C12B C4B 124.2(13) 1_555 1_555 1_555 no N1B C12B C11B 114.9(12) 1_555 1_555 1_555 no C4B C12B C11B 120.9(13) 1_555 1_555 1_555 no Fe N1C C1C 129.9(9) 1_555 1_555 1_555 no Fe N1C C12C 113.7(8) 1_555 1_555 1_555 no C1C N1C C12C 116.3(11) 1_555 1_555 1_555 no Fe N2C C10C 131.0(9) 1_555 1_555 1_555 no Fe N2C C11C 111.5(8) 1_555 1_555 1_555 no C10C N2C C11C 117.4(11) 1_555 1_555 1_555 no N1C C1C C2C 122.0(12) 1_555 1_555 1_555 no C1C C2C C3C 120.3(12) 1_555 1_555 1_555 no C2C C3C C4C 120.4(13) 1_555 1_555 1_555 no C3C C4C C5C 124.9(14) 1_555 1_555 1_555 no C3C C4C C12C 117.5(13) 1_555 1_555 1_555 no C5C C4C C12C 117.6(13) 1_555 1_555 1_555 no C4C C5C C6C 121.5(13) 1_555 1_555 1_555 no C5C C6C C7C 120.5(13) 1_555 1_555 1_555 no C6C C7C C8C 122.6(13) 1_555 1_555 1_555 no C6C C7C C11C 117.5(13) 1_555 1_555 1_555 no C8C C7C C11C 119.9(13) 1_555 1_555 1_555 no C7C C8C C9C 117.6(13) 1_555 1_555 1_555 no C8C C9C C10C 119.5(12) 1_555 1_555 1_555 no N2C C10C C9C 123.8(12) 1_555 1_555 1_555 no N2C C11C C7C 121.7(11) 1_555 1_555 1_555 no N2C C11C C12C 116.8(13) 1_555 1_555 1_555 no C7C C11C C12C 121.4(14) 1_555 1_555 1_555 no N1C C12C C4C 123.5(11) 1_555 1_555 1_555 no N1C C12C C11C 115.1(13) 1_555 1_555 1_555 no C4C C12C C11C 121.4(14) 1_555 1_555 1_555 no I1 Hg I2 109.42(3) 1_555 1_555 1_555 no I1 Hg I3 103.79(4) 1_555 1_555 1_555 no I1 Hg I4 109.84(4) 1_555 1_555 1_555 no I2 Hg I3 113.16(4) 1_555 1_555 1_555 no I2 Hg I4 110.97(4) 1_555 1_555 1_555 no I3 Hg I4 109.40(4) 1_555 1_555 1_555 no N1An C1An C2An 178.4(19) 1_555 1_555 1_555 no O1Et C1Et C2Et 124.8(23) 1_555 1_555 1_555 no data_VMR4_A1-(acetone)(H2O) _database_code_CSD 212710 _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C36 H24 Fe N6 2+,Hg I4 2-,C3 H6 O,H2 O' _chemical_formula_sum 'C39 H32 Fe Hg I4 N6 O2' _chemical_formula_iupac ? _chemical_formula_weight 1380.8 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.200(2) _cell_length_b 13.028(3) _cell_length_c 14.620(3) _cell_angle_alpha 87.378(3) _cell_angle_beta 75.441(3) _cell_angle_gamma 83.887(3) _cell_volume 2053(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 150 _exptl_crystal_description 'thick plates' _exptl_crystal_colour red _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.23 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284.0 _exptl_absorpt_coefficient_mu 7.105 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.637 _exptl_absorpt_correction_T_max 1.000 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_ambient_temperature 150(2) _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 18486 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_max 28.3 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? # REFINEMENT DATA _refine_special_details ? _reflns_number_total 9316 _reflns_number_gt 8694 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.024 _refine_ls_wR_factor_ref 0.037 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8694 _refine_ls_number_parameters 250 _refine_ls_goodness_of_fit_ref 1.28 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.031 _refine_diff_density_max 1.85 _refine_diff_density_min -1.40 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Fe 0.33377(4) 0.25957(4) 0.22715(3) 0.0196(1) Uani Fe 1.0 N1A 0.4751(3) 0.2812(2) 0.1187(2) 0.0213(3) Uani N 1.0 N2A 0.4573(3) 0.1627(2) 0.2705(2) 0.0214(3) Uani N 1.0 C1A 0.4821(3) 0.3424(3) 0.0424(2) 0.0241(3) Uani C 1.0 C2A 0.5929(3) 0.3533(3) -0.0259(2) 0.0285(5) Uani C 1.0 C3A 0.7018(3) 0.2996(3) -0.0149(3) 0.0295(5) Uani C 1.0 C4A 0.6977(3) 0.2333(3) 0.0646(3) 0.0265(3) Uani C 1.0 C5A 0.8036(3) 0.1707(3) 0.0815(3) 0.0301(4) Uani C 1.0 C6A 0.7929(3) 0.1023(3) 0.1556(3) 0.0304(3) Uani C 1.0 C7A 0.6753(3) 0.0956(3) 0.2232(3) 0.0268(3) Uani C 1.0 C8A 0.6573(3) 0.0285(3) 0.3028(3) 0.0301(3) Uani C 1.0 C9A 0.5421(3) 0.0304(3) 0.3636(3) 0.0290(3) Uani C 1.0 C10A 0.4440(3) 0.0988(3) 0.3461(2) 0.0243(3) Uani C 1.0 C11A 0.5726(3) 0.1599(3) 0.2095(2) 0.0227(3) Uani C 1.0 C12A 0.5834(3) 0.2263(3) 0.1286(2) 0.0226(3) Uani C 1.0 N1B 0.1976(3) 0.2292(2) 0.3370(2) 0.0229(3) Uani N 1.0 N2B 0.2785(3) 0.1435(2) 0.1714(2) 0.0225(4) Uani N 1.0 C1B 0.1572(3) 0.2759(3) 0.4196(2) 0.0270(3) Uani C 1.0 C2B 0.0551(3) 0.2457(3) 0.4907(3) 0.0339(5) Uani C 1.0 C3B -0.0060(3) 0.1653(3) 0.4752(3) 0.0357(6) Uani C 1.0 C4B 0.0355(3) 0.1128(3) 0.3890(3) 0.0310(4) Uani C 1.0 C5B -0.0204(4) 0.0272(3) 0.3641(3) 0.0358(5) Uani C 1.0 C6B 0.0234(4) -0.0188(3) 0.2801(3) 0.0351(4) Uani C 1.0 C7B 0.1258(3) 0.0176(3) 0.2093(3) 0.0298(3) Uani C 1.0 C8B 0.1720(4) -0.0230(3) 0.1183(3) 0.0334(3) Uani C 1.0 C9B 0.2697(4) 0.0217(3) 0.0568(3) 0.0319(4) Uani C 1.0 C10B 0.3204(3) 0.1035(3) 0.0860(3) 0.0262(3) Uani C 1.0 C11B 0.1813(3) 0.1015(3) 0.2325(3) 0.0245(3) Uani C 1.0 C12B 0.1371(3) 0.1484(3) 0.3218(2) 0.0249(3) Uani C 1.0 N1C 0.2182(3) 0.3622(2) 0.1814(2) 0.0232(3) Uani N 1.0 N2C 0.3708(3) 0.3808(2) 0.2881(2) 0.0231(4) Uani N 1.0 C1C 0.1435(3) 0.3508(3) 0.1250(3) 0.0273(4) Uani C 1.0 C2C 0.0566(4) 0.4308(3) 0.1073(3) 0.0333(6) Uani C 1.0 C3C 0.0480(4) 0.5258(3) 0.1480(3) 0.0341(6) Uani C 1.0 C4C 0.1287(3) 0.5409(3) 0.2057(3) 0.0295(4) Uani C 1.0 C5C 0.1321(4) 0.6373(3) 0.2492(3) 0.0333(6) Uani C 1.0 C6C 0.2160(4) 0.6484(3) 0.2986(3) 0.0331(5) Uani C 1.0 C7C 0.3028(3) 0.5635(3) 0.3139(3) 0.0292(4) Uani C 1.0 C8C 0.3934(4) 0.5695(3) 0.3649(3) 0.0333(5) Uani C 1.0 C9C 0.4681(4) 0.4822(3) 0.3765(3) 0.0326(5) Uani C 1.0 C10C 0.4539(3) 0.3884(3) 0.3381(3) 0.0270(4) Uani C 1.0 C11C 0.2969(3) 0.4679(3) 0.2753(2) 0.0245(3) Uani C 1.0 C12C 0.2112(3) 0.4575(3) 0.2198(2) 0.0247(3) Uani C 1.0 Hg 0.33388(1) 0.27404(1) -0.21401(1) 0.0262(1) Uani Hg 1.0 I1 0.11436(2) 0.19068(2) -0.10986(2) 0.0308(1) Uani I 1.0 I2 0.31054(2) 0.47053(2) -0.14226(2) 0.0294(1) Uani I 1.0 I3 0.53337(2) 0.14622(2) -0.18103(2) 0.0326(1) Uani I 1.0 I4 0.34291(3) 0.26483(2) -0.40611(2) 0.0406(1) Uani I 1.0 O1Ac 0.7238(4) 0.3071(3) 0.4502(3) 0.091(5) Uani O 1.0 C1Ac 0.7950(3) 0.3471(2) 0.3862(3) 0.046(3) Uani C 1.0 C2Ac 0.8412(5) 0.2990(4) 0.2930(3) 0.058(4) Uani C 1.0 C3Ac 0.8405(5) 0.4468(4) 0.3969(4) 0.066(2) Uani C 1.0 OW1 0.7068(3) 0.1100(3) 0.5652(3) 0.069(1) Uani O 1.0 HC1A 0.4044 0.3826 0.0335 0.025 Uani H 1.0 HC2A 0.5933 0.3996 -0.0824 0.033 Uani H 1.0 HC3A 0.7820 0.3077 -0.0624 0.034 Uani H 1.0 HC5A 0.8870 0.1774 0.0379 0.034 Uani H 1.0 HC6A 0.8673 0.0563 0.1632 0.035 Uani H 1.0 HC8A 0.7276 -0.0198 0.3148 0.035 Uani H 1.0 HC9A 0.5276 -0.0168 0.4203 0.033 Uani H 1.0 HC10A 0.3609 0.0998 0.3919 0.025 Uani H 1.0 HC1B 0.2007 0.3349 0.4320 0.028 Uani H 1.0 HC2B 0.0278 0.2830 0.5518 0.040 Uani H 1.0 HC3B -0.0792 0.1439 0.5244 0.043 Uani H 1.0 HC5B -0.0935 0.0012 0.4103 0.042 Uani H 1.0 HC6B -0.0160 -0.0797 0.2663 0.041 Uani H 1.0 HC8B 0.1357 -0.0826 0.0983 0.040 Uani H 1.0 HC9B 0.3035 -0.0051 -0.0086 0.037 Uani H 1.0 HC10B 0.3914 0.1335 0.0408 0.027 Uani H 1.0 HC1C 0.1495 0.2828 0.0942 0.028 Uani H 1.0 HC2C 0.0013 0.4188 0.0656 0.039 Uani H 1.0 HC3C -0.0140 0.5829 0.1368 0.040 Uani H 1.0 HC5C 0.0707 0.6970 0.2425 0.039 Uani H 1.0 HC6C 0.2183 0.7172 0.3253 0.038 Uani H 1.0 HC8C 0.4028 0.6364 0.3921 0.039 Uani H 1.0 HC9C 0.5329 0.4850 0.4122 0.038 Uani H 1.0 HC10C 0.5081 0.3252 0.3487 0.028 Uani H 1.0 H1C2Ac 0.8044 0.2322 0.2939 0.064 Uani H 1.0 H2C2Ac 0.8170 0.3464 0.2436 0.115 Uani H 1.0 H3C2Ac 0.9336 0.2858 0.2784 0.081 Uani H 1.0 H1C3Ac 0.8033 0.4721 0.4625 0.082 Uani H 1.0 H2C3Ac 0.9329 0.4377 0.3852 0.106 Uani H 1.0 H3C3Ac 0.8163 0.4983 0.3503 0.098 Uani H 1.0 H1OW1 0.7107 0.1770 0.5289 0.069 Uani H 1.0 H2OW1 0.6601 0.1224 0.6323 0.069 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Fe 0.0191(2) 0.0235(2) 0.0161(2) -0.0026(2) -0.0042(2) 0.0012(2) Fe N1A 0.0245(5) 0.0245(6) 0.0148(6) -0.0061(4) -0.0035(4) -0.0002(4) N N2A 0.0249(5) 0.0238(6) 0.0164(5) -0.0044(4) -0.0061(4) 0.0002(4) N C1A 0.0288(5) 0.0276(6) 0.0154(6) -0.0074(4) -0.0028(4) 0.0016(4) C C2A 0.0324(6) 0.0330(9) 0.0179(6) -0.0097(6) 0.0001(5) 0.0017(5) C C3A 0.0290(5) 0.035(1) 0.0217(7) -0.0096(5) 0.0019(5) -0.0018(5) C C4A 0.0246(5) 0.0312(7) 0.0225(6) -0.0067(4) -0.0011(4) -0.0036(5) C C5A 0.0237(5) 0.0350(9) 0.0304(8) -0.0047(4) -0.0025(4) -0.0068(7) C C6A 0.0245(5) 0.0337(9) 0.0331(9) -0.0015(5) -0.0072(4) -0.0063(7) C C7A 0.0259(5) 0.0290(6) 0.0267(7) -0.0016(4) -0.0087(4) -0.0027(5) C C8A 0.0316(6) 0.0306(8) 0.0301(9) 0.0003(6) -0.0130(6) 0.0001(6) C C9A 0.0344(6) 0.0292(8) 0.0251(8) -0.0016(6) -0.0121(6) 0.0034(6) C C10A 0.0297(5) 0.0259(6) 0.0185(6) -0.0040(4) -0.0081(4) 0.0023(5) C C11A 0.0240(5) 0.0255(6) 0.0195(5) -0.0039(4) -0.0060(4) -0.0015(4) C C12A 0.0236(5) 0.0262(5) 0.0180(5) -0.0056(4) -0.0033(4) -0.0019(4) C N1B 0.0200(5) 0.0293(5) 0.0188(6) -0.0009(4) -0.0053(4) 0.0048(4) N N2B 0.0223(5) 0.0253(6) 0.0210(5) -0.0007(4) -0.0087(4) 0.0030(4) N C1B 0.0237(5) 0.0364(6) 0.0190(6) -0.0002(5) -0.0035(5) 0.0030(4) C C2B 0.0270(7) 0.049(1) 0.0218(6) -0.0019(6) -0.0004(6) 0.0050(5) C C3B 0.0255(6) 0.051(1) 0.0270(6) -0.0062(6) -0.0015(6) 0.0112(6) C C4B 0.0235(5) 0.0402(7) 0.0290(6) -0.0071(5) -0.0066(4) 0.0121(5) C C5B 0.0278(7) 0.0423(8) 0.0399(9) -0.0123(7) -0.0124(6) 0.0169(7) C C6B 0.0320(7) 0.0352(7) 0.044(1) -0.0119(7) -0.0186(7) 0.0138(6) C C7B 0.0302(6) 0.0288(6) 0.0351(7) -0.0065(5) -0.0166(5) 0.0071(5) C C8B 0.039(1) 0.0292(7) 0.0389(9) -0.0051(6) -0.0210(7) 0.0015(6) C C9B 0.038(1) 0.0308(7) 0.0311(7) -0.0011(6) -0.0164(6) -0.0029(7) C C10B 0.0282(6) 0.0287(6) 0.0231(5) 0.0002(5) -0.0103(4) -0.0004(5) C C11B 0.0232(5) 0.0268(6) 0.0254(5) -0.0032(4) -0.0105(4) 0.0059(4) C C12B 0.0210(5) 0.0307(5) 0.0233(5) -0.0034(4) -0.0071(4) 0.0077(4) C N1C 0.0228(6) 0.0298(5) 0.0161(6) -0.0034(4) -0.0030(5) 0.0016(4) N N2C 0.0240(6) 0.0291(5) 0.0154(6) -0.0058(4) -0.0022(5) -0.0008(4) N C1C 0.0262(6) 0.0357(5) 0.0206(6) -0.0030(4) -0.0073(5) 0.0022(4) C C2C 0.0301(8) 0.0419(7) 0.029(1) 0.0000(6) -0.0109(7) 0.0047(7) C C3C 0.0305(8) 0.0384(6) 0.031(1) 0.0025(6) -0.0066(7) 0.0062(6) C C4C 0.0285(6) 0.0311(5) 0.0249(7) 0.0001(5) -0.0010(5) 0.0036(4) C C5C 0.0342(9) 0.0293(5) 0.030(1) 0.0002(5) 0.0030(7) 0.0023(5) C C6C 0.0369(9) 0.0281(5) 0.028(1) -0.0040(4) 0.0043(7) -0.0017(5) C C7C 0.0328(7) 0.0291(5) 0.0225(7) -0.0068(4) 0.0011(5) -0.0030(4) C C8C 0.038(1) 0.0344(5) 0.026(1) -0.0110(6) -0.0024(7) -0.0068(6) C C9C 0.0358(9) 0.0385(6) 0.0255(9) -0.0112(6) -0.0072(7) -0.0061(7) C C10C 0.0282(6) 0.0343(5) 0.0196(7) -0.0078(4) -0.0057(5) -0.0025(4) C C11C 0.0260(5) 0.0279(5) 0.0173(6) -0.0051(4) -0.0002(4) -0.0007(4) C C12C 0.0246(5) 0.0286(5) 0.0182(5) -0.0027(4) -0.0009(4) 0.0017(4) C Hg 0.0246(1) 0.0291(1) 0.0252(1) -0.0022(1) -0.0070(1) 0.0000(1) Hg I1 0.0226(1) 0.0294(1) 0.0383(1) -0.0047(1) -0.0032(1) 0.0008(1) I I2 0.0330(1) 0.0271(1) 0.0283(1) -0.0033(1) -0.0076(1) -0.0015(1) I I3 0.0296(1) 0.0364(1) 0.0337(1) 0.0050(1) -0.0141(1) -0.0041(1) I I4 0.0608(2) 0.0386(1) 0.0276(1) -0.0032(1) -0.0219(1) 0.0017(1) I O1Ac 0.098(8) 0.066(3) 0.077(4) -0.022(3) 0.044(4) -0.015(3) O C1Ac 0.041(5) 0.045(3) 0.044(4) 0.004(2) -0.002(2) 0.001(2) C C2Ac 0.081(6) 0.049(2) 0.040(5) 0.002(2) -0.009(2) 0.003(2) C C3Ac 0.075(4) 0.050(2) 0.062(4) -0.008(2) 0.002(3) -0.006(2) C OW1 0.047(2) 0.079(3) 0.067(3) -0.019(2) 0.015(2) 0.001(2) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1A 1.972(3) 1_555 1_555 no Fe N2A 1.976(3) 1_555 1_555 no Fe N1B 1.975(3) 1_555 1_555 no Fe N2B 1.974(3) 1_555 1_555 no Fe N1C 1.974(3) 1_555 1_555 no Fe N2C 1.979(3) 1_555 1_555 no N1A C1A 1.333(4) 1_555 1_555 no N1A C12A 1.377(4) 1_555 1_555 no N2A C10A 1.340(4) 1_555 1_555 no N2A C11A 1.370(4) 1_555 1_555 no C1A C2A 1.400(5) 1_555 1_555 no C2A C3A 1.382(5) 1_555 1_555 no C3A C4A 1.410(5) 1_555 1_555 no C4A C5A 1.434(5) 1_555 1_555 no C4A C12A 1.392(5) 1_555 1_555 no C5A C6A 1.360(6) 1_555 1_555 no C6A C7A 1.443(5) 1_555 1_555 no C7A C8A 1.410(5) 1_555 1_555 no C7A C11A 1.401(5) 1_555 1_555 no C8A C9A 1.369(5) 1_555 1_555 no C9A C10A 1.407(5) 1_555 1_555 no C11A C12A 1.421(5) 1_555 1_555 no N1B C1B 1.329(4) 1_555 1_555 no N1B C12B 1.366(4) 1_555 1_555 no N2B C10B 1.328(4) 1_555 1_555 no N2B C11B 1.369(4) 1_555 1_555 no C1B C2B 1.415(5) 1_555 1_555 no C2B C3B 1.367(6) 1_555 1_555 no C3B C4B 1.410(6) 1_555 1_555 no C4B C5B 1.439(5) 1_555 1_555 no C4B C12B 1.408(5) 1_555 1_555 no C5B C6B 1.345(6) 1_555 1_555 no C6B C7B 1.444(5) 1_555 1_555 no C7B C8B 1.407(6) 1_555 1_555 no C7B C11B 1.406(5) 1_555 1_555 no C8B C9B 1.393(6) 1_555 1_555 no C9B C10B 1.391(5) 1_555 1_555 no C11B C12B 1.417(5) 1_555 1_555 no N1C C1C 1.336(4) 1_555 1_555 no N1C C12C 1.372(4) 1_555 1_555 no N2C C10C 1.333(4) 1_555 1_555 no N2C C11C 1.366(4) 1_555 1_555 no C1C C2C 1.410(5) 1_555 1_555 no C2C C3C 1.381(6) 1_555 1_555 no C3C C4C 1.416(5) 1_555 1_555 no C4C C5C 1.441(5) 1_555 1_555 no C4C C12C 1.392(5) 1_555 1_555 no C5C C6C 1.344(6) 1_555 1_555 no C6C C7C 1.441(5) 1_555 1_555 no C7C C8C 1.412(5) 1_555 1_555 no C7C C11C 1.405(5) 1_555 1_555 no C8C C9C 1.369(6) 1_555 1_555 no C9C C10C 1.407(5) 1_555 1_555 no C11C C12C 1.423(5) 1_555 1_555 no Hg I1 2.842(1) 1_555 1_555 no Hg I2 2.772(1) 1_555 1_555 no Hg I3 2.770(1) 1_555 1_555 no Hg I4 2.792(1) 1_555 1_555 no O1Ac C1Ac 1.204(6) 1_555 1_555 no C1Ac C2Ac 1.473(4) 1_555 1_555 no C1Ac C3Ac 1.473(4) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Fe N2A 83.2(1) 1_555 1_555 1_555 no N1A Fe N1B 176.3(1) 1_555 1_555 1_555 no N1A Fe N2B 95.4(1) 1_555 1_555 1_555 no N1A Fe N1C 94.1(1) 1_555 1_555 1_555 no N1A Fe N2C 89.2(1) 1_555 1_555 1_555 no N2A Fe N1B 93.4(1) 1_555 1_555 1_555 no N2A Fe N2B 89.8(1) 1_555 1_555 1_555 no N2A Fe N1C 176.5(1) 1_555 1_555 1_555 no N2A Fe N2C 94.5(1) 1_555 1_555 1_555 no N1B Fe N2B 83.0(1) 1_555 1_555 1_555 no N1B Fe N1C 89.3(1) 1_555 1_555 1_555 no N1B Fe N2C 92.6(1) 1_555 1_555 1_555 no N2B Fe N1C 92.8(1) 1_555 1_555 1_555 no N2B Fe N2C 174.1(1) 1_555 1_555 1_555 no N1C Fe N2C 83.1(1) 1_555 1_555 1_555 no Fe N1A C1A 130.5(2) 1_555 1_555 1_555 no Fe N1A C12A 112.4(2) 1_555 1_555 1_555 no C1A N1A C12A 117.1(3) 1_555 1_555 1_555 no Fe N2A C10A 130.3(2) 1_555 1_555 1_555 no Fe N2A C11A 112.5(2) 1_555 1_555 1_555 no C10A N2A C11A 117.1(3) 1_555 1_555 1_555 no N1A C1A C2A 123.1(3) 1_555 1_555 1_555 no C1A C2A C3A 119.7(3) 1_555 1_555 1_555 no C2A C3A C4A 118.8(3) 1_555 1_555 1_555 no C3A C4A C5A 123.7(3) 1_555 1_555 1_555 no C3A C4A C12A 117.8(3) 1_555 1_555 1_555 no C5A C4A C12A 118.4(3) 1_555 1_555 1_555 no C4A C5A C6A 121.4(3) 1_555 1_555 1_555 no C5A C6A C7A 120.6(3) 1_555 1_555 1_555 no C6A C7A C8A 124.0(3) 1_555 1_555 1_555 no C6A C7A C11A 118.2(3) 1_555 1_555 1_555 no C8A C7A C11A 117.8(3) 1_555 1_555 1_555 no C7A C8A C9A 118.9(3) 1_555 1_555 1_555 no C8A C9A C10A 120.0(3) 1_555 1_555 1_555 no N2A C10A C9A 122.7(3) 1_555 1_555 1_555 no N2A C11A C7A 123.4(3) 1_555 1_555 1_555 no N2A C11A C12A 116.0(3) 1_555 1_555 1_555 no C7A C11A C12A 120.6(3) 1_555 1_555 1_555 no N1A C12A C4A 123.6(3) 1_555 1_555 1_555 no N1A C12A C11A 115.8(3) 1_555 1_555 1_555 no C4A C12A C11A 120.6(3) 1_555 1_555 1_555 no Fe N1B C1B 130.0(2) 1_555 1_555 1_555 no Fe N1B C12B 112.5(2) 1_555 1_555 1_555 no C1B N1B C12B 117.6(3) 1_555 1_555 1_555 no Fe N2B C10B 129.7(2) 1_555 1_555 1_555 no Fe N2B C11B 112.4(2) 1_555 1_555 1_555 no C10B N2B C11B 117.9(3) 1_555 1_555 1_555 no N1B C1B C2B 122.8(3) 1_555 1_555 1_555 no C1B C2B C3B 119.6(4) 1_555 1_555 1_555 no C2B C3B C4B 119.2(3) 1_555 1_555 1_555 no C3B C4B C5B 124.6(3) 1_555 1_555 1_555 no C3B C4B C12B 117.6(3) 1_555 1_555 1_555 no C5B C4B C12B 117.8(4) 1_555 1_555 1_555 no C4B C5B C6B 121.4(4) 1_555 1_555 1_555 no C5B C6B C7B 121.8(4) 1_555 1_555 1_555 no C6B C7B C8B 124.8(3) 1_555 1_555 1_555 no C6B C7B C11B 117.5(4) 1_555 1_555 1_555 no C8B C7B C11B 117.7(3) 1_555 1_555 1_555 no C7B C8B C9B 118.3(3) 1_555 1_555 1_555 no C8B C9B C10B 120.2(4) 1_555 1_555 1_555 no N2B C10B C9B 122.8(3) 1_555 1_555 1_555 no N2B C11B C7B 123.2(3) 1_555 1_555 1_555 no N2B C11B C12B 116.0(3) 1_555 1_555 1_555 no C7B C11B C12B 120.8(3) 1_555 1_555 1_555 no N1B C12B C4B 123.2(3) 1_555 1_555 1_555 no N1B C12B C11B 116.1(3) 1_555 1_555 1_555 no C4B C12B C11B 120.7(3) 1_555 1_555 1_555 no Fe N1C C1C 130.1(2) 1_555 1_555 1_555 no Fe N1C C12C 112.4(2) 1_555 1_555 1_555 no C1C N1C C12C 117.4(3) 1_555 1_555 1_555 no Fe N2C C10C 130.0(3) 1_555 1_555 1_555 no Fe N2C C11C 112.2(2) 1_555 1_555 1_555 no C10C N2C C11C 117.8(3) 1_555 1_555 1_555 no N1C C1C C2C 122.6(3) 1_555 1_555 1_555 no C1C C2C C3C 119.7(3) 1_555 1_555 1_555 no C2C C3C C4C 118.9(3) 1_555 1_555 1_555 no C3C C4C C5C 124.2(3) 1_555 1_555 1_555 no C3C C4C C12C 117.6(3) 1_555 1_555 1_555 no C5C C4C C12C 118.3(3) 1_555 1_555 1_555 no C4C C5C C6C 121.3(4) 1_555 1_555 1_555 no C5C C6C C7C 121.6(4) 1_555 1_555 1_555 no C6C C7C C8C 124.7(3) 1_555 1_555 1_555 no C6C C7C C11C 117.7(3) 1_555 1_555 1_555 no C8C C7C C11C 117.7(3) 1_555 1_555 1_555 no C7C C8C C9C 118.8(3) 1_555 1_555 1_555 no C8C C9C C10C 120.2(3) 1_555 1_555 1_555 no N2C C10C C9C 122.4(3) 1_555 1_555 1_555 no N2C C11C C7C 123.1(3) 1_555 1_555 1_555 no N2C C11C C12C 116.3(3) 1_555 1_555 1_555 no C7C C11C C12C 120.5(3) 1_555 1_555 1_555 no N1C C12C C4C 123.8(3) 1_555 1_555 1_555 no N1C C12C C11C 115.5(3) 1_555 1_555 1_555 no C4C C12C C11C 120.6(3) 1_555 1_555 1_555 no I1 Hg I2 103.22(1) 1_555 1_555 1_555 no I1 Hg I3 107.41(1) 1_555 1_555 1_555 no I1 Hg I4 108.13(1) 1_555 1_555 1_555 no I2 Hg I3 114.23(1) 1_555 1_555 1_555 no I2 Hg I4 115.82(1) 1_555 1_555 1_555 no I3 Hg I4 107.52(1) 1_555 1_555 1_555 no O1Ac C1Ac C2Ac 121.8(2) 1_555 1_555 1_555 no O1Ac C1Ac C3Ac 121.8(2) 1_555 1_555 1_555 no C2Ac C1Ac C3Ac 116.4(4) 1_555 1_555 1_555 no data_DID255 _database_code_CSD 212711 _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C36 H24 Fe N6 2+,Hg I4 2-,C3 H6 O,H2 O' _chemical_formula_sum 'C39 H32 Fe Hg I4 N6 O2' _chemical_formula_iupac ? _chemical_formula_weight 1380.8 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.384(5) _cell_length_b 12.659(6) _cell_length_c 14.885(7) _cell_angle_alpha 89.37(2) _cell_angle_beta 73.79(3) _cell_angle_gamma 84.19(4) _cell_volume 2049(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 11 _cell_measurement_theta_max 12 _cell_measurement_temperature 294 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.07 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.24 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284.0 _exptl_absorpt_coefficient_mu 7.118 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.13 _exptl_absorpt_correction_T_max 0.47 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 7483 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 7182 _reflns_number_gt 5167 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.050 _refine_ls_wR_factor_ref 0.059 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5167 _refine_ls_number_parameters 246 _refine_ls_goodness_of_fit_ref 1.86 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.011 _refine_diff_density_max 2.42 _refine_diff_density_min -1.99 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Fe 0.32286(12) 0.26744(10) 0.22664(8) 0.0400(3) Uani Fe 1.0 N1A 0.4624(7) 0.2900(6) 0.1178(5) 0.043(1) Uani N 1.0 N2A 0.4492(7) 0.1787(6) 0.2688(5) 0.044(1) Uani N 1.0 C1A 0.4672(10) 0.3454(8) 0.0420(6) 0.052(1) Uani C 1.0 C2A 0.5759(11) 0.3552(9) -0.0275(7) 0.065(2) Uani C 1.0 C3A 0.6849(11) 0.3124(10) -0.0156(8) 0.068(3) Uani C 1.0 C4A 0.6851(10) 0.2538(9) 0.0630(7) 0.059(2) Uani C 1.0 C5A 0.7937(10) 0.1980(10) 0.0818(9) 0.071(2) Uani C 1.0 C6A 0.7855(11) 0.1367(10) 0.1584(9) 0.071(2) Uani C 1.0 C7A 0.6700(10) 0.1264(9) 0.2245(8) 0.061(1) Uani C 1.0 C8A 0.6555(12) 0.0621(10) 0.3018(9) 0.071(2) Uani C 1.0 C9A 0.5415(12) 0.0598(9) 0.3609(8) 0.067(2) Uani C 1.0 C10A 0.4379(10) 0.1178(8) 0.3445(7) 0.053(1) Uani C 1.0 C11A 0.5641(9) 0.1807(8) 0.2087(7) 0.048(1) Uani C 1.0 C12A 0.5723(9) 0.2432(8) 0.1276(6) 0.048(1) Uani C 1.0 N1B 0.1893(7) 0.2330(6) 0.3357(5) 0.045(1) Uani N 1.0 N2B 0.2767(7) 0.1425(6) 0.1709(5) 0.043(1) Uani N 1.0 C1B 0.1486(10) 0.2807(9) 0.4194(7) 0.055(1) Uani C 1.0 C2B 0.0485(11) 0.2483(11) 0.4893(7) 0.070(2) Uani C 1.0 C3B -0.0088(11) 0.1637(11) 0.4725(8) 0.073(3) Uani C 1.0 C4B 0.0319(10) 0.1124(9) 0.3852(7) 0.060(2) Uani C 1.0 C5B -0.0215(11) 0.0233(10) 0.3590(9) 0.068(2) Uani C 1.0 C6B 0.0234(11) -0.0239(9) 0.2746(9) 0.065(2) Uani C 1.0 C7B 0.1256(10) 0.0138(8) 0.2052(7) 0.055(1) Uani C 1.0 C8B 0.1750(11) -0.0294(9) 0.1159(8) 0.062(1) Uani C 1.0 C9B 0.2723(11) 0.0136(9) 0.0559(8) 0.062(1) Uani C 1.0 C10B 0.3220(10) 0.1002(8) 0.0863(7) 0.051(1) Uani C 1.0 C11B 0.1798(9) 0.0999(8) 0.2302(6) 0.046(1) Uani C 1.0 C12B 0.1335(9) 0.1489(8) 0.3188(7) 0.048(1) Uani C 1.0 N1C 0.2034(7) 0.3651(6) 0.1832(5) 0.046(1) Uani N 1.0 N2C 0.3490(7) 0.3986(6) 0.2862(5) 0.046(1) Uani N 1.0 C1C 0.1323(10) 0.3447(9) 0.1294(7) 0.056(1) Uani C 1.0 C2C 0.0475(11) 0.4233(10) 0.1100(8) 0.069(2) Uani C 1.0 C3C 0.0348(11) 0.5239(10) 0.1458(8) 0.068(2) Uani C 1.0 C4C 0.1096(10) 0.5475(8) 0.2019(7) 0.057(1) Uani C 1.0 C5C 0.1096(11) 0.6504(8) 0.2416(7) 0.062(2) Uani C 1.0 C6C 0.1892(11) 0.6683(8) 0.2908(7) 0.061(2) Uani C 1.0 C7C 0.2759(10) 0.5856(8) 0.3077(7) 0.056(1) Uani C 1.0 C8C 0.3581(12) 0.5988(9) 0.3576(8) 0.065(2) Uani C 1.0 C9C 0.4339(12) 0.5136(9) 0.3727(8) 0.067(2) Uani C 1.0 C10C 0.4255(10) 0.4138(8) 0.3358(7) 0.055(1) Uani C 1.0 C11C 0.2737(9) 0.4832(8) 0.2716(6) 0.047(1) Uani C 1.0 C12C 0.1948(9) 0.4662(8) 0.2180(6) 0.048(1) Uani C 1.0 Hg 0.33029(4) 0.26226(4) 0.78618(3) 0.0571(2) Uani Hg 1.0 I1 0.11974(7) 0.17755(6) 0.89783(6) 0.0669(2) Uani I 1.0 I2 0.31203(8) 0.46793(6) 0.85130(6) 0.0672(2) Uani I 1.0 I3 0.53130(7) 0.13819(6) 0.81282(6) 0.0690(2) Uani I 1.0 I4 0.33442(13) 0.24925(9) 0.59864(7) 0.1140(4) Uani I 1.0 O1Ac 0.8940(34) 0.3102(26) 0.3114(17) 0.289(9) Uani O 0.5 C1Ac 0.8170(31) 0.3731(18) 0.3691(15) 0.289(9) Uani C 0.5 C2Ac 0.6847(31) 0.3541(31) 0.4053(18) 0.289(9) Uani C 0.5 C3Ac 0.8527(46) 0.4711(29) 0.4055(34) 0.289(9) Uani C 0.5 O1Ac' 0.7352(40) 0.3048(32) 0.4373(22) 0.289(9) Uani O 0.5 C1Ac' 0.7856(25) 0.3721(19) 0.3799(17) 0.289(9) Uani C 0.5 C2Ac' 0.7814(32) 0.3725(24) 0.2804(17) 0.289(9) Uani C 0.5 C3Ac' 0.8529(50) 0.4561(35) 0.4073(30) 0.289(9) Uani C 0.5 OW 0.6959(13) 0.1095(12) 0.5611(11) 0.171(6) Uani O 1.0 HC1A 0.3889 0.3822 0.0338 0.054 Uani H 1.0 HC2A 0.5739 0.3936 -0.0862 0.077 Uani H 1.0 HC3A 0.7640 0.3234 -0.0633 0.082 Uani H 1.0 HC5A 0.8764 0.2049 0.0373 0.084 Uani H 1.0 HC6A 0.8618 0.0982 0.1685 0.085 Uani H 1.0 HC8A 0.7276 0.0183 0.3137 0.085 Uani H 1.0 HC9A 0.5306 0.0155 0.4181 0.080 Uani H 1.0 HC10A 0.3550 0.1137 0.3896 0.055 Uani H 1.0 HC1B 0.1906 0.3417 0.4330 0.056 Uani H 1.0 HC2B 0.0193 0.2868 0.5510 0.085 Uani H 1.0 HC3B -0.0791 0.1391 0.5222 0.089 Uani H 1.0 HC5B -0.0937 -0.0039 0.4049 0.081 Uani H 1.0 HC6B -0.0148 -0.0867 0.2593 0.075 Uani H 1.0 HC8B 0.1402 -0.0913 0.0955 0.073 Uani H 1.0 HC9B 0.3080 -0.0160 -0.0091 0.074 Uani H 1.0 HC10B 0.3937 0.1302 0.0421 0.055 Uani H 1.0 HC1C 0.1397 0.2716 0.1023 0.059 Uani H 1.0 HC2C -0.0046 0.4055 0.0693 0.083 Uani H 1.0 HC3C -0.0266 0.5795 0.1324 0.080 Uani H 1.0 HC5C 0.0495 0.7100 0.2327 0.071 Uani H 1.0 HC6C 0.1877 0.7414 0.3162 0.069 Uani H 1.0 HC8C 0.3626 0.6706 0.3829 0.076 Uani H 1.0 HC9C 0.4940 0.5222 0.4092 0.081 Uani H 1.0 HC10C 0.4801 0.3515 0.3478 0.059 Uani H 1.0 H1C2Ac 0.6708 0.2870 0.3767 0.289 Uani H 0.5 H2C2Ac 0.6625 0.3477 0.4749 0.289 Uani H 0.5 H3C2Ac 0.6321 0.4150 0.3884 0.289 Uani H 0.5 H1C3Ac 0.9426 0.4761 0.3770 0.289 Uani H 0.5 H2C3Ac 0.8046 0.5350 0.3886 0.289 Uani H 0.5 H3C3Ac 0.8350 0.4677 0.4751 0.289 Uani H 0.5 H1C2Ac' 0.7345 0.3135 0.2696 0.289 Uani H 0.5 H2C2Ac' 0.7398 0.4419 0.2671 0.289 Uani H 0.5 H3C2Ac' 0.8671 0.3623 0.2379 0.289 Uani H 0.5 H1C3Ac' 0.8502 0.4487 0.4748 0.289 Uani H 0.5 H2C3Ac' 0.9405 0.4481 0.3681 0.289 Uani H 0.5 H3C3Ac' 0.8132 0.5278 0.3973 0.289 Uani H 0.5 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Fe 0.0418(8) 0.0405(8) 0.0392(7) -0.0051(6) -0.0135(6) -0.0017(5) Fe N1A 0.050(2) 0.045(2) 0.036(2) -0.012(2) -0.009(1) -0.005(2) N N2A 0.051(2) 0.043(2) 0.041(2) -0.007(1) -0.017(1) -0.004(1) N C1A 0.063(2) 0.054(2) 0.037(2) -0.016(2) -0.007(1) 0.000(2) C C2A 0.075(2) 0.069(4) 0.043(2) -0.024(3) 0.001(2) 0.001(2) C C3A 0.064(2) 0.075(4) 0.055(2) -0.024(2) 0.007(2) -0.010(2) C C4A 0.050(2) 0.064(3) 0.058(2) -0.016(2) -0.002(2) -0.016(2) C C5A 0.046(2) 0.077(4) 0.083(3) -0.010(2) -0.007(1) -0.026(3) C C6A 0.049(2) 0.075(4) 0.091(4) 0.001(2) -0.022(1) -0.025(3) C C7A 0.053(2) 0.061(3) 0.072(3) 0.001(2) -0.026(2) -0.014(2) C C8A 0.071(2) 0.067(3) 0.083(4) 0.008(3) -0.041(2) -0.007(3) C C9A 0.080(3) 0.062(3) 0.067(3) 0.002(3) -0.038(2) 0.004(2) C C10A 0.066(2) 0.050(2) 0.047(2) -0.005(2) -0.024(2) 0.002(2) C C11A 0.048(2) 0.048(2) 0.050(2) -0.005(2) -0.017(1) -0.009(1) C C12A 0.046(2) 0.050(2) 0.046(2) -0.011(2) -0.008(1) -0.010(1) C N1B 0.043(2) 0.049(2) 0.043(2) -0.002(2) -0.014(2) 0.001(1) N N2B 0.045(2) 0.041(2) 0.047(2) 0.000(2) -0.020(1) -0.002(1) N C1B 0.052(2) 0.067(2) 0.043(2) -0.005(2) -0.009(2) -0.004(1) C C2B 0.062(3) 0.094(4) 0.049(2) -0.014(3) -0.003(2) -0.002(2) C C3B 0.060(3) 0.097(4) 0.058(2) -0.021(3) -0.006(2) 0.010(2) C C4B 0.052(2) 0.071(3) 0.061(2) -0.016(2) -0.017(2) 0.014(2) C C5B 0.059(3) 0.073(3) 0.081(3) -0.024(3) -0.028(2) 0.023(3) C C6B 0.063(3) 0.057(3) 0.088(4) -0.020(3) -0.039(2) 0.018(2) C C7B 0.058(2) 0.045(2) 0.072(2) -0.009(2) -0.035(2) 0.005(2) C C8B 0.072(4) 0.047(2) 0.080(3) -0.006(2) -0.041(3) -0.006(2) C C9B 0.072(4) 0.053(3) 0.067(2) -0.002(2) -0.032(2) -0.016(2) C C10B 0.056(2) 0.049(2) 0.051(2) 0.000(2) -0.022(1) -0.010(2) C C11B 0.047(2) 0.042(2) 0.054(2) -0.004(2) -0.024(1) 0.003(1) C C12B 0.045(2) 0.051(2) 0.050(2) -0.006(2) -0.018(1) 0.006(1) C N1C 0.049(2) 0.046(2) 0.045(2) -0.006(1) -0.014(2) -0.001(1) N N2C 0.051(2) 0.043(2) 0.044(2) -0.011(1) -0.013(2) -0.004(1) N C1C 0.058(3) 0.058(2) 0.058(2) -0.005(2) -0.027(2) -0.001(2) C C2C 0.068(3) 0.071(3) 0.075(4) 0.002(2) -0.036(3) 0.002(3) C C3C 0.066(3) 0.066(2) 0.072(4) 0.007(3) -0.025(3) 0.006(2) C C4C 0.059(3) 0.050(2) 0.056(2) 0.001(2) -0.010(2) 0.004(2) C C5C 0.068(4) 0.047(2) 0.058(4) 0.002(2) 0.000(3) 0.004(2) C C6C 0.074(4) 0.042(2) 0.055(3) -0.006(2) 0.003(3) -0.002(1) C C7C 0.068(3) 0.043(2) 0.051(2) -0.012(1) -0.005(2) -0.006(1) C C8C 0.082(4) 0.050(2) 0.064(4) -0.019(2) -0.016(3) -0.013(2) C C9C 0.081(4) 0.058(2) 0.069(4) -0.020(2) -0.029(3) -0.014(2) C C10C 0.063(3) 0.052(2) 0.056(2) -0.014(2) -0.023(2) -0.008(2) C C11C 0.054(2) 0.041(2) 0.044(2) -0.009(1) -0.008(2) -0.003(1) C C12C 0.051(2) 0.044(2) 0.045(2) -0.005(1) -0.009(2) 0.000(1) C Hg 0.0562(3) 0.0566(3) 0.0622(3) -0.0010(2) -0.0243(2) -0.0059(2) Hg I1 0.0499(5) 0.0632(5) 0.0907(5) -0.0086(4) -0.0236(4) -0.0008(4) I I2 0.0736(5) 0.0531(5) 0.0782(5) -0.0090(4) -0.0251(4) -0.0091(4) I I3 0.0633(5) 0.0672(5) 0.0834(5) 0.0103(4) -0.0371(4) -0.0103(4) I I4 0.178(1) 0.1054(8) 0.0754(6) 0.0157(8) -0.0733(7) -0.0137(5) I O1Ac 0.379(9) 0.224(9) 0.183(9) 0.055(9) 0.022(9) 0.076(9) O C1Ac 0.379(9) 0.224(9) 0.183(9) 0.055(9) 0.022(9) 0.076(9) C C2Ac 0.379(9) 0.224(9) 0.183(9) 0.055(9) 0.022(9) 0.076(9) C C3Ac 0.379(9) 0.224(9) 0.183(9) 0.055(9) 0.022(9) 0.076(9) C O1Ac' 0.379(9) 0.224(9) 0.183(9) 0.055(9) 0.022(9) 0.076(9) O C1Ac' 0.379(9) 0.224(9) 0.183(9) 0.055(9) 0.022(9) 0.076(9) C C2Ac' 0.379(9) 0.224(9) 0.183(9) 0.055(9) 0.022(9) 0.076(9) C C3Ac' 0.379(9) 0.224(9) 0.183(9) 0.055(9) 0.022(9) 0.076(9) C OW 0.126(9) 0.160(9) 0.185(9) -0.061(9) 0.040(9) -0.030(9) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1A 1.968(7) 1_555 1_555 no Fe N2A 1.972(8) 1_555 1_555 no Fe N1B 1.970(7) 1_555 1_555 no Fe N2B 1.976(8) 1_555 1_555 no Fe N1C 1.983(8) 1_555 1_555 no Fe N2C 1.977(8) 1_555 1_555 no N1A C1A 1.313(12) 1_555 1_555 no N1A C12A 1.374(12) 1_555 1_555 no N2A C10A 1.341(11) 1_555 1_555 no N2A C11A 1.366(12) 1_555 1_555 no C1A C2A 1.389(14) 1_555 1_555 no C2A C3A 1.360(17) 1_555 1_555 no C3A C4A 1.379(16) 1_555 1_555 no C4A C5A 1.456(16) 1_555 1_555 no C4A C12A 1.391(14) 1_555 1_555 no C5A C6A 1.359(17) 1_555 1_555 no C6A C7A 1.422(16) 1_555 1_555 no C7A C8A 1.384(16) 1_555 1_555 no C7A C11A 1.403(14) 1_555 1_555 no C8A C9A 1.352(17) 1_555 1_555 no C9A C10A 1.404(15) 1_555 1_555 no C11A C12A 1.421(14) 1_555 1_555 no N1B C1B 1.330(12) 1_555 1_555 no N1B C12B 1.353(12) 1_555 1_555 no N2B C10B 1.318(11) 1_555 1_555 no N2B C11B 1.361(12) 1_555 1_555 no C1B C2B 1.404(15) 1_555 1_555 no C2B C3B 1.368(17) 1_555 1_555 no C3B C4B 1.395(16) 1_555 1_555 no C4B C5B 1.440(16) 1_555 1_555 no C4B C12B 1.410(14) 1_555 1_555 no C5B C6B 1.340(16) 1_555 1_555 no C6B C7B 1.442(16) 1_555 1_555 no C7B C8B 1.385(15) 1_555 1_555 no C7B C11B 1.406(14) 1_555 1_555 no C8B C9B 1.371(16) 1_555 1_555 no C9B C10B 1.416(14) 1_555 1_555 no C11B C12B 1.403(13) 1_555 1_555 no N1C C1C 1.331(12) 1_555 1_555 no N1C C12C 1.370(12) 1_555 1_555 no N2C C10C 1.319(12) 1_555 1_555 no N2C C11C 1.358(12) 1_555 1_555 no C1C C2C 1.401(15) 1_555 1_555 no C2C C3C 1.364(16) 1_555 1_555 no C3C C4C 1.403(16) 1_555 1_555 no C4C C5C 1.436(15) 1_555 1_555 no C4C C12C 1.407(14) 1_555 1_555 no C5C C6C 1.350(16) 1_555 1_555 no C6C C7C 1.434(15) 1_555 1_555 no C7C C8C 1.370(16) 1_555 1_555 no C7C C11C 1.413(13) 1_555 1_555 no C8C C9C 1.368(16) 1_555 1_555 no C9C C10C 1.405(14) 1_555 1_555 no C11C C12C 1.390(14) 1_555 1_555 no Hg I1 2.813(1) 1_555 1_555 no Hg I2 2.756(1) 1_555 1_555 no Hg I3 2.762(1) 1_555 1_555 no Hg I4 2.785(1) 1_555 1_555 no O1Ac C1Ac 1.262(23) 1_555 1_555 no C1Ac C2Ac 1.495(12) 1_555 1_555 no C1Ac C3Ac 1.495(12) 1_555 1_555 no O1Ac' C1Ac' 1.262(23) 1_555 1_555 no C1Ac' C2Ac' 1.495(12) 1_555 1_555 no C1Ac' C3Ac' 1.495(12) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Fe N2A 83.2(3) 1_555 1_555 1_555 no N1A Fe N1B 175.4(3) 1_555 1_555 1_555 no N1A Fe N2B 94.7(3) 1_555 1_555 1_555 no N1A Fe N1C 94.3(3) 1_555 1_555 1_555 no N1A Fe N2C 89.7(3) 1_555 1_555 1_555 no N2A Fe N1B 93.0(3) 1_555 1_555 1_555 no N2A Fe N2B 91.4(3) 1_555 1_555 1_555 no N2A Fe N1C 175.9(3) 1_555 1_555 1_555 no N2A Fe N2C 93.9(3) 1_555 1_555 1_555 no N1B Fe N2B 82.6(3) 1_555 1_555 1_555 no N1B Fe N1C 89.5(3) 1_555 1_555 1_555 no N1B Fe N2C 93.3(3) 1_555 1_555 1_555 no N2B Fe N1C 92.1(3) 1_555 1_555 1_555 no N2B Fe N2C 173.5(3) 1_555 1_555 1_555 no N1C Fe N2C 82.8(3) 1_555 1_555 1_555 no Fe N1A C1A 130.8(7) 1_555 1_555 1_555 no Fe N1A C12A 112.4(6) 1_555 1_555 1_555 no C1A N1A C12A 116.7(8) 1_555 1_555 1_555 no Fe N2A C10A 130.0(7) 1_555 1_555 1_555 no Fe N2A C11A 112.4(6) 1_555 1_555 1_555 no C10A N2A C11A 117.6(8) 1_555 1_555 1_555 no N1A C1A C2A 123.1(10) 1_555 1_555 1_555 no C1A C2A C3A 119.9(10) 1_555 1_555 1_555 no C2A C3A C4A 119.2(10) 1_555 1_555 1_555 no C3A C4A C5A 125.1(11) 1_555 1_555 1_555 no C3A C4A C12A 117.7(11) 1_555 1_555 1_555 no C5A C4A C12A 117.2(10) 1_555 1_555 1_555 no C4A C5A C6A 121.6(11) 1_555 1_555 1_555 no C5A C6A C7A 121.0(11) 1_555 1_555 1_555 no C6A C7A C8A 123.5(11) 1_555 1_555 1_555 no C6A C7A C11A 118.5(11) 1_555 1_555 1_555 no C8A C7A C11A 117.9(11) 1_555 1_555 1_555 no C7A C8A C9A 118.5(11) 1_555 1_555 1_555 no C8A C9A C10A 122.1(10) 1_555 1_555 1_555 no N2A C10A C9A 120.5(10) 1_555 1_555 1_555 no N2A C11A C7A 123.3(9) 1_555 1_555 1_555 no N2A C11A C12A 116.2(9) 1_555 1_555 1_555 no C7A C11A C12A 120.6(10) 1_555 1_555 1_555 no N1A C12A C4A 123.3(9) 1_555 1_555 1_555 no N1A C12A C11A 115.6(8) 1_555 1_555 1_555 no C4A C12A C11A 121.1(10) 1_555 1_555 1_555 no Fe N1B C1B 129.3(7) 1_555 1_555 1_555 no Fe N1B C12B 112.4(6) 1_555 1_555 1_555 no C1B N1B C12B 118.4(8) 1_555 1_555 1_555 no Fe N2B C10B 129.6(7) 1_555 1_555 1_555 no Fe N2B C11B 112.3(6) 1_555 1_555 1_555 no C10B N2B C11B 118.0(8) 1_555 1_555 1_555 no N1B C1B C2B 122.2(10) 1_555 1_555 1_555 no C1B C2B C3B 119.7(10) 1_555 1_555 1_555 no C2B C3B C4B 119.2(10) 1_555 1_555 1_555 no C3B C4B C5B 124.4(11) 1_555 1_555 1_555 no C3B C4B C12B 117.8(11) 1_555 1_555 1_555 no C5B C4B C12B 117.8(10) 1_555 1_555 1_555 no C4B C5B C6B 121.5(11) 1_555 1_555 1_555 no C5B C6B C7B 121.3(11) 1_555 1_555 1_555 no C6B C7B C8B 124.6(10) 1_555 1_555 1_555 no C6B C7B C11B 117.8(10) 1_555 1_555 1_555 no C8B C7B C11B 117.7(10) 1_555 1_555 1_555 no C7B C8B C9B 119.3(10) 1_555 1_555 1_555 no C8B C9B C10B 119.7(10) 1_555 1_555 1_555 no N2B C10B C9B 122.1(10) 1_555 1_555 1_555 no N2B C11B C7B 123.3(9) 1_555 1_555 1_555 no N2B C11B C12B 115.8(9) 1_555 1_555 1_555 no C7B C11B C12B 120.9(9) 1_555 1_555 1_555 no N1B C12B C4B 122.6(9) 1_555 1_555 1_555 no N1B C12B C11B 116.8(9) 1_555 1_555 1_555 no C4B C12B C11B 120.6(10) 1_555 1_555 1_555 no Fe N1C C1C 129.4(7) 1_555 1_555 1_555 no Fe N1C C12C 111.9(6) 1_555 1_555 1_555 no C1C N1C C12C 118.7(9) 1_555 1_555 1_555 no Fe N2C C10C 130.1(7) 1_555 1_555 1_555 no Fe N2C C11C 111.8(6) 1_555 1_555 1_555 no C10C N2C C11C 118.1(8) 1_555 1_555 1_555 no N1C C1C C2C 121.4(10) 1_555 1_555 1_555 no C1C C2C C3C 121.0(11) 1_555 1_555 1_555 no C2C C3C C4C 118.6(10) 1_555 1_555 1_555 no C3C C4C C5C 124.8(10) 1_555 1_555 1_555 no C3C C4C C12C 118.2(10) 1_555 1_555 1_555 no C5C C4C C12C 116.9(10) 1_555 1_555 1_555 no C4C C5C C6C 121.3(10) 1_555 1_555 1_555 no C5C C6C C7C 121.9(10) 1_555 1_555 1_555 no C6C C7C C8C 124.5(10) 1_555 1_555 1_555 no C6C C7C C11C 117.1(10) 1_555 1_555 1_555 no C8C C7C C11C 118.3(10) 1_555 1_555 1_555 no C7C C8C C9C 120.0(10) 1_555 1_555 1_555 no C8C C9C C10C 118.7(10) 1_555 1_555 1_555 no N2C C10C C9C 123.0(10) 1_555 1_555 1_555 no N2C C11C C7C 121.9(9) 1_555 1_555 1_555 no N2C C11C C12C 117.4(8) 1_555 1_555 1_555 no C7C C11C C12C 120.6(10) 1_555 1_555 1_555 no N1C C12C C4C 122.0(9) 1_555 1_555 1_555 no N1C C12C C11C 116.0(9) 1_555 1_555 1_555 no C4C C12C C11C 122.0(9) 1_555 1_555 1_555 no I1 Hg I2 104.95(3) 1_555 1_555 1_555 no I1 Hg I3 106.80(3) 1_555 1_555 1_555 no I1 Hg I4 109.54(4) 1_555 1_555 1_555 no I2 Hg I3 112.84(3) 1_555 1_555 1_555 no I2 Hg I4 113.30(3) 1_555 1_555 1_555 no I3 Hg I4 109.10(3) 1_555 1_555 1_555 no O1Ac C1Ac C2Ac 122.00(2) 1_555 1_555 1_555 no O1Ac C1Ac C3Ac 122.00(2) 1_555 1_555 1_555 no C2Ac C1Ac C3Ac 116.00(1) 1_555 1_555 1_555 no O1Ac' C1Ac' C2Ac' 122.00(1) 1_555 1_555 1_555 no O1Ac' C1Ac' C3Ac' 122.00(3) 1_555 1_555 1_555 no C2Ac' C1Ac' C3Ac' 116.00(1) 1_555 1_555 1_555 no data_DID261_B-(dmf)2 _database_code_CSD 212712 _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C36 H24 Fe N6 2+,Hg I4 2-,2(C3 H7 N O)' _chemical_formula_sum 'C42 H38 Fe Hg I4 N8 O2' _chemical_formula_iupac ? _chemical_formula_weight 1450.9 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.585(6) _cell_length_b 12.543(7) _cell_length_c 17.013(8) _cell_angle_alpha 70.16(3) _cell_angle_beta 76.87(3) _cell_angle_gamma 84.26(3) _cell_volume 2264(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description rhomboid _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.13 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360.0 _exptl_absorpt_coefficient_mu 6.448 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.27 _exptl_absorpt_correction_T_max 0.53 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 5755 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_max 22 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 24 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 5526 _reflns_number_gt 4065 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.035 _refine_ls_wR_factor_ref 0.043 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4065 _refine_ls_number_parameters 265 _refine_ls_goodness_of_fit_ref 1.40 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.011 _refine_diff_density_max 1.49 _refine_diff_density_min -1.77 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Fe 0.54547(10) 0.63796(10) 0.71372(8) 0.0376(3) Uani Fe 1.0 N1A 0.6901(6) 0.5601(6) 0.6695(4) 0.039(1) Uani N 1.0 N2A 0.4859(6) 0.4817(6) 0.7629(4) 0.040(1) Uani N 1.0 C1A 0.7943(7) 0.6044(8) 0.6209(6) 0.046(1) Uani C 1.0 C2A 0.8894(8) 0.5344(9) 0.5986(6) 0.055(2) Uani C 1.0 C3A 0.8789(8) 0.4202(9) 0.6264(6) 0.056(2) Uani C 1.0 C4A 0.7716(8) 0.3715(8) 0.6751(6) 0.049(1) Uani C 1.0 C5A 0.7494(9) 0.2544(8) 0.7043(6) 0.057(2) Uani C 1.0 C6A 0.6390(9) 0.2142(8) 0.7490(7) 0.058(2) Uani C 1.0 C7A 0.5444(9) 0.2885(8) 0.7678(6) 0.052(1) Uani C 1.0 C8A 0.4280(9) 0.2532(8) 0.8104(7) 0.060(2) Uani C 1.0 C9A 0.3469(9) 0.3310(8) 0.8308(7) 0.058(2) Uani C 1.0 C10A 0.3790(8) 0.4438(8) 0.8069(6) 0.047(1) Uani C 1.0 C11A 0.5679(8) 0.4032(7) 0.7436(6) 0.043(1) Uani C 1.0 C12A 0.6801(8) 0.4458(7) 0.6946(6) 0.042(1) Uani C 1.0 N1B 0.4723(6) 0.6599(6) 0.6155(5) 0.042(1) Uani N 1.0 N2B 0.3954(6) 0.7068(6) 0.7562(5) 0.042(1) Uani N 1.0 C1B 0.5159(9) 0.6381(8) 0.5423(6) 0.053(1) Uani C 1.0 C2B 0.4492(10) 0.6571(9) 0.4798(7) 0.069(2) Uani C 1.0 C3B 0.3349(10) 0.6964(9) 0.4944(7) 0.072(1) Uani C 1.0 C4B 0.2866(9) 0.7223(8) 0.5683(7) 0.062(1) Uani C 1.0 C5B 0.1715(10) 0.7693(9) 0.5856(8) 0.075(2) Uani C 1.0 C6B 0.1328(9) 0.7968(9) 0.6574(9) 0.076(2) Uani C 1.0 C7B 0.2041(8) 0.7794(8) 0.7185(8) 0.064(2) Uani C 1.0 C8B 0.1716(9) 0.8057(9) 0.7950(8) 0.076(3) Uani C 1.0 C9B 0.2486(9) 0.7836(9) 0.8489(8) 0.071(2) Uani C 1.0 C10B 0.3607(8) 0.7329(8) 0.8288(7) 0.054(1) Uani C 1.0 C11B 0.3168(8) 0.7307(7) 0.7025(6) 0.048(1) Uani C 1.0 C12B 0.3596(8) 0.7047(7) 0.6265(6) 0.047(1) Uani C 1.0 N1C 0.6201(6) 0.7865(6) 0.6655(5) 0.039(1) Uani N 1.0 N2C 0.6126(6) 0.6276(6) 0.8124(5) 0.040(1) Uani N 1.0 C1C 0.6247(8) 0.8649(7) 0.5902(6) 0.045(1) Uani C 1.0 C2C 0.6856(8) 0.9655(8) 0.5630(6) 0.055(2) Uani C 1.0 C3C 0.7475(8) 0.9859(8) 0.6169(7) 0.056(2) Uani C 1.0 C4C 0.7460(8) 0.9059(8) 0.6971(7) 0.051(1) Uani C 1.0 C5C 0.8088(8) 0.9153(9) 0.7586(7) 0.060(2) Uani C 1.0 C6C 0.8036(8) 0.8318(9) 0.8360(7) 0.063(2) Uani C 1.0 C7C 0.7379(8) 0.7324(9) 0.8586(7) 0.055(1) Uani C 1.0 C8C 0.7321(9) 0.6413(10) 0.9342(7) 0.065(2) Uani C 1.0 C9C 0.6686(9) 0.5499(9) 0.9482(7) 0.062(2) Uani C 1.0 C10C 0.6086(8) 0.5444(8) 0.8862(6) 0.049(1) Uani C 1.0 C11C 0.6773(7) 0.7203(8) 0.7985(6) 0.043(1) Uani C 1.0 C12C 0.6818(7) 0.8068(7) 0.7194(6) 0.042(1) Uani C 1.0 Hg 0.81711(4) 0.82337(4) 0.32004(3) 0.0595(2) Uani Hg 1.0 I1 0.94717(5) 0.86096(6) 0.42915(5) 0.0583(2) Uani I 1.0 I2 0.60254(6) 0.93914(6) 0.33630(5) 0.0644(2) Uani I 1.0 I3 0.78529(6) 0.59184(6) 0.36738(5) 0.0682(2) Uani I 1.0 I4 0.95696(8) 0.91253(8) 0.15687(6) 0.0983(3) Uani I 1.0 O1D1 0.5864(11) 0.2821(6) 0.9745(7) 0.162(9) Uani O 1.0 N1D1 0.6360(6) 0.1001(6) 1.0092(5) 0.084(5) Uani N 1.0 C1D1 0.6517(8) 0.2002(11) 0.9617(6) 0.113(7) Uani C 1.0 C2D1 0.5401(11) 0.0724(10) 1.0829(7) 0.097(5) Uani C 1.0 C3D1 0.7095(11) 0.0096(12) 0.9942(10) 0.146(6) Uani C 1.0 O1D2 1.1274(9) 0.5047(11) 0.9087(9) 0.200(5) Uani O 1.0 N1D2 0.9878(6) 0.4256(7) 0.8795(5) 0.097(7) Uani N 1.0 C1D2 1.0594(10) 0.5026(9) 0.8609(6) 0.136(6) Uani C 1.0 C2D2 0.9792(15) 0.3329(12) 0.9586(8) 0.184(9) Uani C 1.0 C3D2 0.9124(11) 0.4244(14) 0.8254(10) 0.162(9) Uani C 1.0 HC1A 0.8040 0.6884 0.6004 0.048 Uani H 1.0 HC2A 0.9657 0.5690 0.5620 0.065 Uani H 1.0 HC3A 0.9481 0.3709 0.6119 0.065 Uani H 1.0 HC5A 0.8147 0.1999 0.6925 0.065 Uani H 1.0 HC6A 0.6253 0.1309 0.7685 0.067 Uani H 1.0 HC8A 0.4056 0.1727 0.8254 0.071 Uani H 1.0 HC9A 0.2648 0.3076 0.8627 0.069 Uani H 1.0 HC10A 0.3184 0.4990 0.8236 0.049 Uani H 1.0 HC1B 0.5989 0.6072 0.5322 0.056 Uani H 1.0 HC2B 0.4847 0.6421 0.4250 0.085 Uani H 1.0 HC3B 0.2853 0.7067 0.4512 0.089 Uani H 1.0 HC5B 0.1183 0.7824 0.5443 0.092 Uani H 1.0 HC6B 0.0511 0.8305 0.6679 0.094 Uani H 1.0 HC8B 0.0918 0.8408 0.8098 0.094 Uani H 1.0 HC9B 0.2255 0.8034 0.9027 0.088 Uani H 1.0 HC10B 0.4157 0.7158 0.8694 0.056 Uani H 1.0 HC1C 0.5815 0.8512 0.5500 0.048 Uani H 1.0 HC2C 0.6846 1.0223 0.5053 0.065 Uani H 1.0 HC3C 0.7926 1.0572 0.5984 0.066 Uani H 1.0 HC5C 0.8567 0.9838 0.7445 0.069 Uani H 1.0 HC6C 0.8473 0.8411 0.8776 0.075 Uani H 1.0 HC8C 0.7752 0.6437 0.9782 0.079 Uani H 1.0 HC9C 0.6639 0.4854 1.0030 0.075 Uani H 1.0 HC10C 0.5617 0.4759 0.8983 0.050 Uani H 1.0 HC1D1 0.7191 0.2165 0.9111 0.164 Uani H 1.0 H1C2D1 0.4947 0.1433 1.0866 0.149 Uani H 1.0 H2C2D1 0.4861 0.0190 1.0775 0.104 Uani H 1.0 H3C2D1 0.5729 0.0359 1.1356 0.129 Uani H 1.0 H1C3D1 0.7723 0.0394 0.9416 0.221 Uani H 1.0 H2C3D1 0.7476 -0.0290 1.0442 0.194 Uani H 1.0 H3C3D1 0.6609 -0.0459 0.9861 0.148 Uani H 1.0 HC1D2 1.0631 0.5657 0.8054 0.235 Uani H 1.0 H1C2D2 1.0368 0.3433 0.9911 0.223 Uani H 1.0 H2C2D2 0.8969 0.3311 0.9934 0.299 Uani H 1.0 H3C2D2 0.9981 0.2599 0.9463 0.231 Uani H 1.0 H1C3D2 0.9266 0.4927 0.7730 0.232 Uani H 1.0 H2C3D2 0.9292 0.3542 0.8089 0.152 Uani H 1.0 H3C3D2 0.8280 0.4255 0.8561 0.283 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Fe 0.0379(7) 0.0330(7) 0.0430(8) -0.0015(6) -0.0104(6) -0.0125(6) Fe N1A 0.041(2) 0.039(2) 0.040(2) -0.001(1) -0.011(2) -0.013(1) N N2A 0.045(2) 0.035(2) 0.041(2) -0.006(1) -0.011(2) -0.011(2) N C1A 0.041(2) 0.047(2) 0.049(3) -0.002(1) -0.007(2) -0.017(2) C C2A 0.044(2) 0.059(2) 0.060(4) 0.003(2) -0.006(2) -0.023(3) C C3A 0.052(2) 0.058(2) 0.060(4) 0.011(2) -0.012(2) -0.024(3) C C4A 0.056(2) 0.045(2) 0.051(3) 0.009(2) -0.016(2) -0.019(2) C C5A 0.073(3) 0.043(2) 0.057(4) 0.012(2) -0.020(3) -0.020(2) C C6A 0.080(3) 0.036(2) 0.058(4) 0.004(1) -0.019(3) -0.016(2) C C7A 0.067(2) 0.035(2) 0.053(3) -0.005(1) -0.014(2) -0.013(2) C C8A 0.075(3) 0.038(2) 0.065(4) -0.015(2) -0.009(3) -0.014(2) C C9A 0.063(2) 0.044(2) 0.065(4) -0.018(2) -0.004(2) -0.014(2) C C10A 0.049(2) 0.041(2) 0.051(3) -0.011(2) -0.007(2) -0.013(2) C C11A 0.052(2) 0.035(2) 0.043(2) -0.003(1) -0.013(1) -0.012(2) C C12A 0.047(2) 0.038(2) 0.042(2) 0.002(1) -0.014(1) -0.014(1) C N1B 0.050(2) 0.032(2) 0.043(2) -0.013(1) -0.014(2) -0.006(2) N N2B 0.043(2) 0.031(2) 0.051(2) -0.008(2) -0.007(2) -0.010(2) N C1B 0.068(2) 0.049(3) 0.043(2) -0.017(2) -0.015(2) -0.012(2) C C2B 0.094(4) 0.069(4) 0.050(2) -0.025(3) -0.029(2) -0.012(2) C C3B 0.090(3) 0.066(4) 0.065(3) -0.025(3) -0.043(3) -0.003(3) C C4B 0.064(2) 0.048(3) 0.071(3) -0.016(2) -0.036(2) 0.001(2) C C5B 0.062(2) 0.055(4) 0.104(4) -0.013(2) -0.046(3) 0.004(3) C C6B 0.049(2) 0.052(4) 0.117(5) -0.004(2) -0.032(2) -0.004(4) C C7B 0.044(2) 0.044(2) 0.094(3) -0.002(2) -0.015(2) -0.012(3) C C8B 0.051(2) 0.059(4) 0.109(4) 0.003(2) -0.001(2) -0.028(4) C C9B 0.061(2) 0.062(4) 0.087(3) -0.001(2) 0.006(2) -0.034(3) C C10B 0.055(2) 0.045(2) 0.060(2) -0.007(2) -0.001(2) -0.022(2) C C11B 0.043(2) 0.033(2) 0.064(2) -0.007(2) -0.013(2) -0.007(2) C C12B 0.049(2) 0.034(2) 0.056(2) -0.012(1) -0.021(2) -0.003(2) C N1C 0.034(2) 0.032(2) 0.047(2) 0.003(2) -0.005(2) -0.012(1) N N2C 0.036(2) 0.039(2) 0.044(2) 0.004(1) -0.010(2) -0.013(1) N C1C 0.044(2) 0.034(2) 0.051(2) 0.001(2) -0.006(2) -0.008(2) C C2C 0.054(3) 0.036(2) 0.064(3) -0.005(2) -0.004(2) -0.007(2) C C3C 0.050(3) 0.039(2) 0.075(3) -0.007(2) -0.001(3) -0.017(2) C C4C 0.041(2) 0.043(2) 0.069(3) -0.004(2) -0.004(2) -0.024(2) C C5C 0.047(3) 0.059(3) 0.083(4) -0.008(2) -0.009(3) -0.037(2) C C6C 0.052(3) 0.072(3) 0.079(3) -0.006(3) -0.018(3) -0.039(3) C C7C 0.050(2) 0.063(3) 0.062(2) -0.001(2) -0.018(2) -0.027(2) C C8C 0.066(3) 0.078(4) 0.060(2) -0.002(3) -0.028(3) -0.023(2) C C9C 0.067(4) 0.069(3) 0.052(2) 0.000(3) -0.025(2) -0.013(2) C C10C 0.049(2) 0.048(2) 0.046(2) 0.002(2) -0.015(2) -0.010(1) C C11C 0.038(2) 0.045(2) 0.051(2) 0.002(1) -0.010(1) -0.019(1) C C12C 0.035(2) 0.038(2) 0.054(2) 0.001(1) -0.006(1) -0.018(1) C Hg 0.0512(3) 0.0555(3) 0.0729(3) 0.0013(2) -0.0158(2) -0.0213(2) Hg I1 0.0457(4) 0.0631(5) 0.0703(5) -0.0025(3) -0.0154(3) -0.0249(4) I I2 0.0498(4) 0.0570(5) 0.0819(6) 0.0062(3) -0.0153(4) -0.0179(4) I I3 0.0658(5) 0.0519(5) 0.0904(6) -0.0048(4) -0.0214(4) -0.0234(4) I I4 0.1070(7) 0.0946(7) 0.0747(6) 0.0022(5) 0.0135(5) -0.0262(5) I O1D1 0.281(9) 0.064(6) 0.147(9) -0.020(7) -0.089(9) -0.009(4) O N1D1 0.089(9) 0.075(5) 0.082(6) -0.019(5) -0.021(5) -0.010(4) N C1D1 0.163(9) 0.088(6) 0.085(8) -0.054(7) -0.038(6) 0.001(5) C C2D1 0.119(9) 0.081(6) 0.082(8) -0.020(6) -0.007(4) -0.022(4) C C3D1 0.101(9) 0.131(7) 0.183(9) 0.013(5) -0.001(9) -0.046(8) C O1D2 0.142(9) 0.261(9) 0.268(9) -0.035(9) -0.042(9) -0.170(9) O N1D2 0.064(9) 0.136(9) 0.091(9) -0.008(8) 0.008(7) -0.051(7) N C1D2 0.141(9) 0.139(9) 0.133(9) -0.041(7) -0.003(8) -0.057(7) C C2D2 0.261(9) 0.183(9) 0.081(8) -0.066(9) 0.026(9) -0.032(8) C C3D2 0.102(9) 0.236(9) 0.210(9) 0.050(9) -0.065(9) -0.146(9) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1A 1.981(7) 1_555 1_555 no Fe N2A 1.978(7) 1_555 1_555 no Fe N1B 1.967(7) 1_555 1_555 no Fe N2B 1.960(7) 1_555 1_555 no Fe N1C 1.963(7) 1_555 1_555 no Fe N2C 1.966(7) 1_555 1_555 no N1A C1A 1.348(10) 1_555 1_555 no N1A C12A 1.358(11) 1_555 1_555 no N2A C10A 1.332(10) 1_555 1_555 no N2A C11A 1.368(10) 1_555 1_555 no C1A C2A 1.405(12) 1_555 1_555 no C2A C3A 1.356(13) 1_555 1_555 no C3A C4A 1.395(13) 1_555 1_555 no C4A C5A 1.412(13) 1_555 1_555 no C4A C12A 1.399(12) 1_555 1_555 no C5A C6A 1.376(13) 1_555 1_555 no C6A C7A 1.419(13) 1_555 1_555 no C7A C8A 1.413(13) 1_555 1_555 no C7A C11A 1.392(12) 1_555 1_555 no C8A C9A 1.361(13) 1_555 1_555 no C9A C10A 1.396(13) 1_555 1_555 no C11A C12A 1.419(12) 1_555 1_555 no N1B C1B 1.341(11) 1_555 1_555 no N1B C12B 1.367(11) 1_555 1_555 no N2B C10B 1.349(11) 1_555 1_555 no N2B C11B 1.375(11) 1_555 1_555 no C1B C2B 1.397(13) 1_555 1_555 no C2B C3B 1.364(15) 1_555 1_555 no C3B C4B 1.386(15) 1_555 1_555 no C4B C5B 1.413(15) 1_555 1_555 no C4B C12B 1.393(12) 1_555 1_555 no C5B C6B 1.347(16) 1_555 1_555 no C6B C7B 1.419(15) 1_555 1_555 no C7B C8B 1.410(15) 1_555 1_555 no C7B C11B 1.394(13) 1_555 1_555 no C8B C9B 1.365(15) 1_555 1_555 no C9B C10B 1.410(13) 1_555 1_555 no C11B C12B 1.410(13) 1_555 1_555 no N1C C1C 1.317(11) 1_555 1_555 no N1C C12C 1.382(11) 1_555 1_555 no N2C C10C 1.327(11) 1_555 1_555 no N2C C11C 1.370(11) 1_555 1_555 no C1C C2C 1.392(12) 1_555 1_555 no C2C C3C 1.383(14) 1_555 1_555 no C3C C4C 1.391(13) 1_555 1_555 no C4C C5C 1.443(14) 1_555 1_555 no C4C C12C 1.406(12) 1_555 1_555 no C5C C6C 1.369(14) 1_555 1_555 no C6C C7C 1.418(14) 1_555 1_555 no C7C C8C 1.393(14) 1_555 1_555 no C7C C11C 1.421(13) 1_555 1_555 no C8C C9C 1.347(14) 1_555 1_555 no C9C C10C 1.411(13) 1_555 1_555 no C11C C12C 1.406(12) 1_555 1_555 no Hg I1 2.819(1) 1_555 1_555 no Hg I2 2.757(1) 1_555 1_555 no Hg I3 2.777(1) 1_555 1_555 no Hg I4 2.792(1) 1_555 1_555 no O1D1 C1D1 1.262(11) 1_555 1_555 no N1D1 C1D1 1.246(11) 1_555 1_555 no N1D1 C2D1 1.440(11) 1_555 1_555 no N1D1 C3D1 1.409(12) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Fe N2A 82.3(3) 1_555 1_555 1_555 no N1A Fe N1B 94.6(3) 1_555 1_555 1_555 no N1A Fe N2B 175.7(3) 1_555 1_555 1_555 no N1A Fe N1C 92.8(3) 1_555 1_555 1_555 no N1A Fe N2C 89.3(3) 1_555 1_555 1_555 no N2A Fe N1B 88.8(3) 1_555 1_555 1_555 no N2A Fe N2B 94.2(3) 1_555 1_555 1_555 no N2A Fe N1C 174.4(3) 1_555 1_555 1_555 no N2A Fe N2C 94.3(3) 1_555 1_555 1_555 no N1B Fe N2B 82.8(3) 1_555 1_555 1_555 no N1B Fe N1C 94.3(3) 1_555 1_555 1_555 no N1B Fe N2C 175.4(3) 1_555 1_555 1_555 no N2B Fe N1C 90.8(3) 1_555 1_555 1_555 no N2B Fe N2C 93.5(3) 1_555 1_555 1_555 no N1C Fe N2C 83.0(3) 1_555 1_555 1_555 no Fe N1A C1A 129.2(6) 1_555 1_555 1_555 no Fe N1A C12A 113.2(6) 1_555 1_555 1_555 no C1A N1A C12A 117.6(7) 1_555 1_555 1_555 no Fe N2A C10A 130.3(6) 1_555 1_555 1_555 no Fe N2A C11A 112.9(6) 1_555 1_555 1_555 no C10A N2A C11A 116.7(8) 1_555 1_555 1_555 no N1A C1A C2A 121.0(9) 1_555 1_555 1_555 no C1A C2A C3A 120.6(9) 1_555 1_555 1_555 no C2A C3A C4A 120.1(9) 1_555 1_555 1_555 no C3A C4A C5A 124.8(9) 1_555 1_555 1_555 no C3A C4A C12A 116.5(9) 1_555 1_555 1_555 no C5A C4A C12A 118.7(9) 1_555 1_555 1_555 no C4A C5A C6A 120.9(9) 1_555 1_555 1_555 no C5A C6A C7A 121.3(9) 1_555 1_555 1_555 no C6A C7A C8A 124.1(9) 1_555 1_555 1_555 no C6A C7A C11A 118.0(9) 1_555 1_555 1_555 no C8A C7A C11A 117.9(9) 1_555 1_555 1_555 no C7A C8A C9A 118.7(9) 1_555 1_555 1_555 no C8A C9A C10A 119.7(9) 1_555 1_555 1_555 no N2A C10A C9A 123.6(9) 1_555 1_555 1_555 no N2A C11A C7A 123.3(8) 1_555 1_555 1_555 no N2A C11A C12A 115.8(8) 1_555 1_555 1_555 no C7A C11A C12A 120.9(8) 1_555 1_555 1_555 no N1A C12A C4A 124.2(8) 1_555 1_555 1_555 no N1A C12A C11A 115.7(8) 1_555 1_555 1_555 no C4A C12A C11A 120.1(8) 1_555 1_555 1_555 no Fe N1B C1B 130.1(6) 1_555 1_555 1_555 no Fe N1B C12B 112.4(6) 1_555 1_555 1_555 no C1B N1B C12B 117.5(8) 1_555 1_555 1_555 no Fe N2B C10B 129.2(6) 1_555 1_555 1_555 no Fe N2B C11B 113.4(6) 1_555 1_555 1_555 no C10B N2B C11B 117.4(8) 1_555 1_555 1_555 no N1B C1B C2B 122.2(9) 1_555 1_555 1_555 no C1B C2B C3B 119.0(10) 1_555 1_555 1_555 no C2B C3B C4B 120.9(10) 1_555 1_555 1_555 no C3B C4B C5B 124.1(10) 1_555 1_555 1_555 no C3B C4B C12B 116.8(10) 1_555 1_555 1_555 no C5B C4B C12B 119.0(11) 1_555 1_555 1_555 no C4B C5B C6B 120.6(10) 1_555 1_555 1_555 no C5B C6B C7B 122.1(10) 1_555 1_555 1_555 no C6B C7B C8B 126.2(10) 1_555 1_555 1_555 no C6B C7B C11B 117.4(11) 1_555 1_555 1_555 no C8B C7B C11B 116.3(10) 1_555 1_555 1_555 no C7B C8B C9B 120.3(10) 1_555 1_555 1_555 no C8B C9B C10B 120.0(11) 1_555 1_555 1_555 no N2B C10B C9B 121.5(10) 1_555 1_555 1_555 no N2B C11B C7B 124.4(10) 1_555 1_555 1_555 no N2B C11B C12B 114.6(8) 1_555 1_555 1_555 no C7B C11B C12B 121.0(9) 1_555 1_555 1_555 no N1B C12B C4B 123.5(10) 1_555 1_555 1_555 no N1B C12B C11B 116.7(8) 1_555 1_555 1_555 no C4B C12B C11B 119.8(9) 1_555 1_555 1_555 no Fe N1C C1C 130.5(6) 1_555 1_555 1_555 no Fe N1C C12C 112.8(6) 1_555 1_555 1_555 no C1C N1C C12C 116.7(8) 1_555 1_555 1_555 no Fe N2C C10C 130.1(6) 1_555 1_555 1_555 no Fe N2C C11C 112.5(6) 1_555 1_555 1_555 no C10C N2C C11C 117.3(8) 1_555 1_555 1_555 no N1C C1C C2C 124.3(9) 1_555 1_555 1_555 no C1C C2C C3C 119.1(9) 1_555 1_555 1_555 no C2C C3C C4C 119.1(9) 1_555 1_555 1_555 no C3C C4C C5C 124.7(9) 1_555 1_555 1_555 no C3C C4C C12C 118.0(9) 1_555 1_555 1_555 no C5C C4C C12C 117.3(9) 1_555 1_555 1_555 no C4C C5C C6C 121.0(9) 1_555 1_555 1_555 no C5C C6C C7C 121.6(10) 1_555 1_555 1_555 no C6C C7C C8C 125.4(10) 1_555 1_555 1_555 no C6C C7C C11C 118.4(10) 1_555 1_555 1_555 no C8C C7C C11C 116.1(9) 1_555 1_555 1_555 no C7C C8C C9C 120.3(10) 1_555 1_555 1_555 no C8C C9C C10C 120.6(10) 1_555 1_555 1_555 no N2C C10C C9C 121.9(9) 1_555 1_555 1_555 no N2C C11C C7C 123.8(9) 1_555 1_555 1_555 no N2C C11C C12C 116.4(8) 1_555 1_555 1_555 no C7C C11C C12C 119.8(9) 1_555 1_555 1_555 no N1C C12C C4C 122.9(8) 1_555 1_555 1_555 no N1C C12C C11C 115.2(8) 1_555 1_555 1_555 no C4C C12C C11C 121.9(9) 1_555 1_555 1_555 no I1 Hg I2 108.29(3) 1_555 1_555 1_555 no I1 Hg I3 108.36(3) 1_555 1_555 1_555 no I1 Hg I4 104.32(3) 1_555 1_555 1_555 no I2 Hg I3 111.16(3) 1_555 1_555 1_555 no I2 Hg I4 111.40(3) 1_555 1_555 1_555 no I3 Hg I4 112.94(3) 1_555 1_555 1_555 no C1D1 N1D1 C2D1 120.5(6) 1_555 1_555 1_555 no C1D1 N1D1 C3D1 122.5(8) 1_555 1_555 1_555 no C2D1 N1D1 C3D1 117.0(8) 1_555 1_555 1_555 no O1D1 C1D1 N1D1 123.1(6) 1_555 1_555 1_555 no data_DID254_C-(acetone) _database_code_CSD 212713 _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C36 H24 Fe N6 2+,Hg I4 2-,C3 H6 O' _chemical_formula_sum 'C39 H30 Fe Hg I4 N6 O' _chemical_formula_iupac ? _chemical_formula_weight 1362.8 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z _cell_length_a 9.709(4) _cell_length_b 9.885(4) _cell_length_c 10.814(5) _cell_angle_alpha 76.06(2) _cell_angle_beta 83.63(2) _cell_angle_gamma 87.07(3) _cell_volume 1000.8(7) _cell_formula_units_Z 1 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 13 _cell_measurement_theta_max 16 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.26 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632.0 _exptl_absorpt_coefficient_mu 7.283 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.30 _exptl_absorpt_correction_T_max 0.63 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 3730 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 3730 _reflns_number_gt 2792 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.061 _refine_ls_wR_factor_ref 0.068 _refine_ls_abs_structure_details ; The enantiomer was confirmed, the alternative giving R,wR 0.076,0.089 ; _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2792 _refine_ls_number_parameters 234 _refine_ls_goodness_of_fit_ref 1.96 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 3.28 _refine_diff_density_min -2.28 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Fe 0.5000 0.5000 0.5000 0.0344(8) Uani Fe 1.0 N1A 0.5783(20) 0.6398(20) 0.5728(20) 0.039(3) Uani N 1.0 N2A 0.5451(20) 0.3716(20) 0.6629(19) 0.039(3) Uani N 1.0 C1A 0.5909(26) 0.7775(26) 0.5334(26) 0.044(3) Uani C 1.0 C2A 0.6519(26) 0.8650(28) 0.5919(29) 0.052(4) Uani C 1.0 C3A 0.7023(28) 0.8018(30) 0.7058(29) 0.053(4) Uani C 1.0 C4A 0.6904(26) 0.6649(29) 0.7554(26) 0.048(3) Uani C 1.0 C5A 0.7463(28) 0.5863(32) 0.8751(27) 0.055(3) Uani C 1.0 C6A 0.7341(28) 0.4455(33) 0.9143(27) 0.055(3) Uani C 1.0 C7A 0.6685(27) 0.3647(30) 0.8485(26) 0.049(3) Uani C 1.0 C8A 0.6395(28) 0.2219(30) 0.8909(27) 0.054(3) Uani C 1.0 C9A 0.5708(28) 0.1625(28) 0.8241(27) 0.052(3) Uani C 1.0 C10A 0.5252(25) 0.2381(26) 0.7095(25) 0.044(3) Uani C 1.0 C11A 0.6095(25) 0.4375(28) 0.7317(25) 0.041(3) Uani C 1.0 C12A 0.6296(24) 0.5829(26) 0.6895(24) 0.041(2) Uani C 1.0 N1B 0.6784(20) 0.4534(20) 0.4158(18) 0.037(3) Uani N 1.0 N2B 0.4425(20) 0.3434(20) 0.4379(19) 0.037(3) Uani N 1.0 C1B 0.8046(25) 0.5138(27) 0.4066(24) 0.044(3) Uani C 1.0 C2B 0.9221(27) 0.4649(31) 0.3411(27) 0.054(4) Uani C 1.0 C3B 0.9212(29) 0.3551(31) 0.2875(27) 0.057(5) Uani C 1.0 C4B 0.7948(29) 0.2924(28) 0.2944(25) 0.050(3) Uani C 1.0 C5B 0.7779(33) 0.1775(31) 0.2434(28) 0.058(4) Uani C 1.0 C6B 0.6481(32) 0.1176(28) 0.2546(26) 0.059(3) Uani C 1.0 C7B 0.5339(31) 0.1734(27) 0.3224(26) 0.050(3) Uani C 1.0 C8B 0.3925(34) 0.1183(29) 0.3378(28) 0.059(3) Uani C 1.0 C9B 0.2920(31) 0.1700(29) 0.4019(28) 0.056(3) Uani C 1.0 C10B 0.3136(26) 0.2867(26) 0.4506(24) 0.045(3) Uani C 1.0 C11B 0.5436(26) 0.2793(25) 0.3710(23) 0.041(3) Uani C 1.0 C12B 0.6784(26) 0.3443(26) 0.3604(23) 0.040(3) Uani C 1.0 N1C 0.4517(19) 0.6387(20) 0.3455(18) 0.035(3) Uani N 1.0 N2C 0.3137(19) 0.5455(20) 0.5630(18) 0.037(3) Uani N 1.0 C1C 0.5296(25) 0.6780(27) 0.2308(23) 0.042(3) Uani C 1.0 C2C 0.4746(28) 0.7824(29) 0.1302(25) 0.051(3) Uani C 1.0 C3C 0.3468(28) 0.8417(28) 0.1449(26) 0.052(3) Uani C 1.0 C4C 0.2716(26) 0.8031(26) 0.2614(26) 0.046(3) Uani C 1.0 C5C 0.1312(28) 0.8575(30) 0.2900(29) 0.056(5) Uani C 1.0 C6C 0.0543(28) 0.8088(32) 0.4092(32) 0.060(5) Uani C 1.0 C7C 0.1160(26) 0.7059(30) 0.5032(28) 0.052(3) Uani C 1.0 C8C 0.0418(29) 0.6465(34) 0.6236(31) 0.063(4) Uani C 1.0 C9C 0.1030(28) 0.5433(34) 0.7067(29) 0.059(3) Uani C 1.0 C10C 0.2368(25) 0.4964(28) 0.6767(25) 0.045(3) Uani C 1.0 C11C 0.2480(24) 0.6499(26) 0.4803(24) 0.040(3) Uani C 1.0 C12C 0.3277(24) 0.6994(25) 0.3576(24) 0.038(3) Uani C 1.0 Hg 0.0575(4) 0.0323(4) 0.8435(3) 0.0553(4) Uani Hg 1.0 I1 -0.1401(4) -0.1197(4) 1.0316(4) 0.0527(5) Uani I 1.0 I2 -0.0700(4) 0.1630(5) 0.6297(4) 0.0871(8) Uani I 1.0 I3 0.2925(4) -0.1024(4) 0.7563(4) 0.0644(6) Uani I 1.0 I4 0.1450(4) 0.2057(4) 0.9896(4) 0.0668(6) Uani I 1.0 O1Ac 0.2503(21) 0.4831(25) 0.2161(23) 0.087(9) Uani O 1.0 C1Ac 0.2600(18) 0.5192(19) 0.0958(33) 0.065(9) Uani C 1.0 C2Ac 0.1366(34) 0.5912(35) 0.0320(33) 0.089(9) Uani C 1.0 C3Ac 0.3945(38) 0.4885(39) 0.0221(33) 0.095(9) Uani C 1.0 HC1A 0.5513 0.8228 0.4515 0.045 Uani H 1.0 HC2A 0.6590 0.9674 0.5539 0.058 Uani H 1.0 HC3A 0.7487 0.8593 0.7527 0.061 Uani H 1.0 HC5A 0.7932 0.6372 0.9274 0.063 Uani H 1.0 HC6A 0.7744 0.3965 0.9949 0.063 Uani H 1.0 HC8A 0.6722 0.1664 0.9729 0.063 Uani H 1.0 HC9A 0.5501 0.0611 0.8551 0.059 Uani H 1.0 HC10A 0.4741 0.1876 0.6596 0.045 Uani H 1.0 HC1B 0.8128 0.5935 0.4472 0.047 Uani H 1.0 HC2B 1.0112 0.5140 0.3336 0.065 Uani H 1.0 HC3B 1.0077 0.3204 0.2446 0.068 Uani H 1.0 HC5B 0.8598 0.1376 0.1983 0.068 Uani H 1.0 HC6B 0.6359 0.0374 0.2158 0.069 Uani H 1.0 HC8B 0.3748 0.0402 0.2981 0.070 Uani H 1.0 HC9B 0.1985 0.1274 0.4172 0.067 Uani H 1.0 HC10B 0.2333 0.3292 0.4954 0.047 Uani H 1.0 HC1C 0.6236 0.6349 0.2167 0.045 Uani H 1.0 HC2C 0.5327 0.8124 0.0465 0.060 Uani H 1.0 HC3C 0.3088 0.9114 0.0726 0.061 Uani H 1.0 HC5C 0.0892 0.9310 0.2231 0.065 Uani H 1.0 HC6C -0.0417 0.8460 0.4272 0.072 Uani H 1.0 HC8C -0.0542 0.6808 0.6462 0.077 Uani H 1.0 HC9C 0.0513 0.5000 0.7911 0.071 Uani H 1.0 HC10C 0.2793 0.4220 0.7426 0.047 Uani H 1.0 H1C2Ac 0.0593 0.6007 0.0988 0.113 Uani H 1.0 H2C2Ac 0.1632 0.6858 -0.0205 0.121 Uani H 1.0 H3C2Ac 0.1056 0.5348 -0.0247 0.109 Uani H 1.0 H1C3Ac 0.4615 0.4406 0.0834 0.114 Uani H 1.0 H2C3Ac 0.3767 0.4269 -0.0351 0.143 Uani H 1.0 H3C3Ac 0.4344 0.5778 -0.0310 0.109 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Fe 0.031(2) 0.040(2) 0.032(2) -0.005(2) -0.003(2) -0.006(2) Fe N1A 0.030(5) 0.044(5) 0.043(4) -0.004(4) 0.000(4) -0.012(4) N N2A 0.031(5) 0.045(5) 0.039(5) -0.002(4) 0.000(4) -0.007(4) N C1A 0.036(5) 0.044(5) 0.052(5) -0.005(4) -0.001(4) -0.014(4) C C2A 0.043(9) 0.050(5) 0.066(8) -0.007(6) -0.004(7) -0.022(5) C C3A 0.042(8) 0.060(5) 0.064(8) -0.006(7) -0.005(7) -0.028(6) C C4A 0.037(6) 0.062(5) 0.051(5) -0.004(5) -0.004(4) -0.023(5) C C5A 0.042(8) 0.078(9) 0.051(6) -0.002(7) -0.008(6) -0.026(6) C C6A 0.043(8) 0.079(9) 0.044(5) 0.001(7) -0.008(5) -0.017(5) C C7A 0.039(6) 0.064(5) 0.041(5) 0.000(5) -0.005(4) -0.009(4) C C8A 0.047(9) 0.064(6) 0.044(5) 0.001(6) -0.006(5) 0.000(5) C C9A 0.046(9) 0.054(5) 0.048(5) -0.001(5) -0.003(5) 0.002(5) C C10A 0.037(6) 0.046(5) 0.045(5) -0.003(4) -0.001(4) -0.004(4) C C11A 0.032(5) 0.052(4) 0.039(5) -0.002(4) -0.001(4) -0.010(4) C C12A 0.032(5) 0.052(4) 0.043(4) -0.003(4) -0.002(3) -0.015(4) C N1B 0.039(5) 0.041(5) 0.027(5) -0.007(4) -0.001(4) -0.002(4) N N2B 0.045(5) 0.037(5) 0.028(5) -0.011(4) -0.002(4) -0.003(4) N C1B 0.039(5) 0.055(6) 0.036(6) -0.010(4) 0.001(4) -0.006(4) C C2B 0.041(5) 0.073(9) 0.047(9) -0.007(4) 0.004(5) -0.012(7) C C3B 0.048(5) 0.073(9) 0.047(8) 0.002(5) 0.005(5) -0.013(7) C C4B 0.054(5) 0.055(6) 0.038(5) 0.003(5) 0.002(5) -0.009(4) C C5B 0.073(7) 0.056(7) 0.044(7) 0.007(6) 0.003(6) -0.015(6) C C6B 0.083(9) 0.049(6) 0.045(8) -0.002(6) 0.001(7) -0.016(6) C C7B 0.070(6) 0.043(5) 0.039(6) -0.010(4) -0.001(5) -0.011(4) C C8B 0.080(8) 0.050(6) 0.049(9) -0.023(6) -0.002(7) -0.017(6) C C9B 0.068(6) 0.055(7) 0.049(9) -0.028(6) -0.001(7) -0.015(6) C C10B 0.051(5) 0.047(5) 0.037(6) -0.019(4) -0.002(4) -0.008(4) C C11B 0.053(4) 0.038(5) 0.030(5) -0.008(3) -0.002(3) -0.005(4) C C12B 0.047(4) 0.042(5) 0.030(5) -0.003(4) -0.001(4) -0.004(4) C N1C 0.030(4) 0.044(5) 0.032(5) -0.012(3) -0.004(3) -0.010(4) N N2C 0.028(4) 0.049(5) 0.035(4) -0.009(4) 0.000(3) -0.012(4) N C1C 0.038(4) 0.054(6) 0.032(5) -0.013(4) -0.002(3) -0.007(4) C C2C 0.049(7) 0.063(8) 0.037(5) -0.014(6) -0.007(4) 0.000(5) C C3C 0.049(7) 0.058(7) 0.045(5) -0.012(6) -0.014(5) 0.000(5) C C4C 0.040(5) 0.051(6) 0.048(5) -0.008(4) -0.013(4) -0.006(4) C C5C 0.042(6) 0.058(7) 0.067(8) -0.001(6) -0.017(5) -0.007(6) C C6C 0.037(5) 0.067(8) 0.073(9) 0.004(6) -0.009(5) -0.012(6) C C7C 0.032(4) 0.064(6) 0.058(6) 0.000(4) -0.002(3) -0.014(5) C C8C 0.035(5) 0.083(9) 0.065(8) 0.004(5) 0.008(4) -0.014(7) C C9C 0.036(5) 0.083(9) 0.053(6) -0.002(5) 0.011(5) -0.011(6) C C10C 0.032(4) 0.063(6) 0.040(5) -0.008(4) 0.005(4) -0.011(4) C C11C 0.029(4) 0.050(5) 0.042(4) -0.007(3) -0.003(3) -0.013(4) C C12C 0.032(4) 0.045(5) 0.039(4) -0.009(3) -0.007(3) -0.010(4) C Hg 0.0470(7) 0.0673(8) 0.0464(7) -0.0063(6) -0.0031(6) -0.0032(6) Hg I1 0.045(1) 0.059(1) 0.053(1) -0.0128(9) 0.0022(9) -0.011(1) I I2 0.055(1) 0.129(2) 0.054(1) -0.001(1) -0.007(1) 0.023(1) I I3 0.053(1) 0.067(1) 0.067(1) -0.009(1) 0.015(1) -0.013(1) I I4 0.087(2) 0.051(1) 0.061(1) -0.023(1) 0.003(1) -0.011(1) I O1Ac 0.085(9) 0.105(9) 0.064(9) -0.039(9) 0.003(9) -0.006(9) O C1Ac 0.077(9) 0.052(9) 0.064(9) -0.028(9) 0.003(9) -0.009(9) C C2Ac 0.079(9) 0.081(9) 0.090(9) -0.029(9) -0.001(9) 0.015(9) C C3Ac 0.088(9) 0.105(9) 0.086(9) -0.015(9) 0.014(9) -0.019(9) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1A 1.968(20) 1_555 1_555 no Fe N2A 1.986(20) 1_555 1_555 no Fe N1B 1.953(20) 1_555 1_555 no Fe N2B 1.958(19) 1_555 1_555 no Fe N1C 1.974(19) 1_555 1_555 no Fe N2C 1.931(19) 1_555 1_555 no N1A C1A 1.332(30) 1_555 1_555 no N1A C12A 1.387(31) 1_555 1_555 no N2A C10A 1.311(29) 1_555 1_555 no N2A C11A 1.322(31) 1_555 1_555 no C1A C2A 1.378(36) 1_555 1_555 no C2A C3A 1.370(39) 1_555 1_555 no C3A C4A 1.336(37) 1_555 1_555 no C4A C5A 1.484(39) 1_555 1_555 no C4A C12A 1.391(34) 1_555 1_555 no C5A C6A 1.361(40) 1_555 1_555 no C6A C7A 1.406(39) 1_555 1_555 no C7A C8A 1.408(38) 1_555 1_555 no C7A C11A 1.457(36) 1_555 1_555 no C8A C9A 1.289(38) 1_555 1_555 no C9A C10A 1.391(36) 1_555 1_555 no C11A C12A 1.416(34) 1_555 1_555 no N1B C1B 1.374(30) 1_555 1_555 no N1B C12B 1.355(30) 1_555 1_555 no N2B C10B 1.377(30) 1_555 1_555 no N2B C11B 1.375(30) 1_555 1_555 no C1B C2B 1.402(36) 1_555 1_555 no C2B C3B 1.349(39) 1_555 1_555 no C3B C4B 1.389(38) 1_555 1_555 no C4B C5B 1.401(38) 1_555 1_555 no C4B C12B 1.409(35) 1_555 1_555 no C5B C6B 1.401(42) 1_555 1_555 no C6B C7B 1.422(38) 1_555 1_555 no C7B C8B 1.481(41) 1_555 1_555 no C7B C11B 1.291(34) 1_555 1_555 no C8B C9B 1.290(41) 1_555 1_555 no C9B C10B 1.412(36) 1_555 1_555 no C11B C12B 1.468(35) 1_555 1_555 no N1C C1C 1.360(31) 1_555 1_555 no N1C C12C 1.325(29) 1_555 1_555 no N2C C10C 1.361(30) 1_555 1_555 no N2C C11C 1.374(30) 1_555 1_555 no C1C C2C 1.437(35) 1_555 1_555 no C2C C3C 1.354(37) 1_555 1_555 no C3C C4C 1.364(37) 1_555 1_555 no C4C C5C 1.468(37) 1_555 1_555 no C4C C12C 1.408(33) 1_555 1_555 no C5C C6C 1.405(43) 1_555 1_555 no C6C C7C 1.415(38) 1_555 1_555 no C7C C8C 1.424(41) 1_555 1_555 no C7C C11C 1.390(34) 1_555 1_555 no C8C C9C 1.348(41) 1_555 1_555 no C9C C10C 1.388(35) 1_555 1_555 no C11C C12C 1.448(34) 1_555 1_555 no Hg I1 2.834(2) 1_555 1_555 no Hg I2 2.753(2) 1_555 1_555 no Hg I3 2.772(2) 1_555 1_555 no Hg I4 2.812(2) 1_555 1_555 no O1Ac C1Ac 1.257(37) 1_555 1_555 no C1Ac C2Ac 1.510(30) 1_555 1_555 no C1Ac C3Ac 1.510(30) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Fe N2A 82.9(8) 1_555 1_555 1_555 no N1A Fe N1B 93.7(8) 1_555 1_555 1_555 no N1A Fe N2B 172.1(8) 1_555 1_555 1_555 no N1A Fe N1C 93.5(8) 1_555 1_555 1_555 no N1A Fe N2C 91.8(8) 1_555 1_555 1_555 no N2A Fe N1B 90.1(8) 1_555 1_555 1_555 no N2A Fe N2B 90.8(8) 1_555 1_555 1_555 no N2A Fe N1C 175.6(8) 1_555 1_555 1_555 no N2A Fe N2C 95.6(8) 1_555 1_555 1_555 no N1B Fe N2B 81.4(8) 1_555 1_555 1_555 no N1B Fe N1C 92.7(8) 1_555 1_555 1_555 no N1B Fe N2C 172.6(8) 1_555 1_555 1_555 no N2B Fe N1C 93.0(8) 1_555 1_555 1_555 no N2B Fe N2C 93.7(8) 1_555 1_555 1_555 no N1C Fe N2C 82.0(8) 1_555 1_555 1_555 no Fe N1A C1A 133.1(17) 1_555 1_555 1_555 no Fe N1A C12A 113.1(15) 1_555 1_555 1_555 no C1A N1A C12A 113.8(20) 1_555 1_555 1_555 no Fe N2A C10A 131.7(17) 1_555 1_555 1_555 no Fe N2A C11A 111.0(16) 1_555 1_555 1_555 no C10A N2A C11A 117.3(21) 1_555 1_555 1_555 no N1A C1A C2A 127.8(24) 1_555 1_555 1_555 no C1A C2A C3A 115.4(24) 1_555 1_555 1_555 no C2A C3A C4A 121.2(25) 1_555 1_555 1_555 no C3A C4A C5A 125.3(25) 1_555 1_555 1_555 no C3A C4A C12A 120.1(25) 1_555 1_555 1_555 no C5A C4A C12A 114.6(24) 1_555 1_555 1_555 no C4A C5A C6A 120.6(24) 1_555 1_555 1_555 no C5A C6A C7A 124.1(25) 1_555 1_555 1_555 no C6A C7A C8A 126.7(26) 1_555 1_555 1_555 no C6A C7A C11A 117.4(25) 1_555 1_555 1_555 no C8A C7A C11A 115.5(24) 1_555 1_555 1_555 no C7A C8A C9A 120.2(26) 1_555 1_555 1_555 no C8A C9A C10A 120.6(26) 1_555 1_555 1_555 no N2A C10A C9A 123.8(24) 1_555 1_555 1_555 no N2A C11A C7A 122.3(24) 1_555 1_555 1_555 no N2A C11A C12A 120.2(22) 1_555 1_555 1_555 no C7A C11A C12A 117.4(23) 1_555 1_555 1_555 no N1A C12A C4A 121.6(23) 1_555 1_555 1_555 no N1A C12A C11A 112.6(21) 1_555 1_555 1_555 no C4A C12A C11A 125.7(24) 1_555 1_555 1_555 no Fe N1B C1B 129.3(17) 1_555 1_555 1_555 no Fe N1B C12B 115.4(16) 1_555 1_555 1_555 no C1B N1B C12B 115.3(21) 1_555 1_555 1_555 no Fe N2B C10B 129.5(17) 1_555 1_555 1_555 no Fe N2B C11B 116.5(16) 1_555 1_555 1_555 no C10B N2B C11B 114.0(20) 1_555 1_555 1_555 no N1B C1B C2B 120.7(24) 1_555 1_555 1_555 no C1B C2B C3B 123.5(26) 1_555 1_555 1_555 no C2B C3B C4B 117.1(25) 1_555 1_555 1_555 no C3B C4B C5B 123.6(26) 1_555 1_555 1_555 no C3B C4B C12B 118.1(25) 1_555 1_555 1_555 no C5B C4B C12B 118.3(26) 1_555 1_555 1_555 no C4B C5B C6B 121.0(26) 1_555 1_555 1_555 no C5B C6B C7B 118.6(25) 1_555 1_555 1_555 no C6B C7B C8B 122.4(25) 1_555 1_555 1_555 no C6B C7B C11B 122.9(27) 1_555 1_555 1_555 no C8B C7B C11B 114.6(26) 1_555 1_555 1_555 no C7B C8B C9B 120.7(25) 1_555 1_555 1_555 no C8B C9B C10B 120.1(26) 1_555 1_555 1_555 no N2B C10B C9B 121.7(24) 1_555 1_555 1_555 no N2B C11B C7B 128.9(25) 1_555 1_555 1_555 no N2B C11B C12B 111.5(20) 1_555 1_555 1_555 no C7B C11B C12B 119.6(25) 1_555 1_555 1_555 no N1B C12B C4B 125.3(23) 1_555 1_555 1_555 no N1B C12B C11B 115.2(21) 1_555 1_555 1_555 no C4B C12B C11B 119.5(23) 1_555 1_555 1_555 no Fe N1C C1C 128.0(16) 1_555 1_555 1_555 no Fe N1C C12C 114.6(16) 1_555 1_555 1_555 no C1C N1C C12C 117.4(20) 1_555 1_555 1_555 no Fe N2C C10C 131.7(17) 1_555 1_555 1_555 no Fe N2C C11C 114.6(15) 1_555 1_555 1_555 no C10C N2C C11C 113.7(20) 1_555 1_555 1_555 no N1C C1C C2C 119.0(23) 1_555 1_555 1_555 no C1C C2C C3C 122.3(25) 1_555 1_555 1_555 no C2C C3C C4C 117.8(24) 1_555 1_555 1_555 no C3C C4C C5C 123.5(24) 1_555 1_555 1_555 no C3C C4C C12C 118.5(24) 1_555 1_555 1_555 no C5C C4C C12C 117.8(24) 1_555 1_555 1_555 no C4C C5C C6C 121.6(24) 1_555 1_555 1_555 no C5C C6C C7C 118.3(24) 1_555 1_555 1_555 no C6C C7C C8C 121.4(24) 1_555 1_555 1_555 no C6C C7C C11C 122.2(26) 1_555 1_555 1_555 no C8C C7C C11C 116.2(25) 1_555 1_555 1_555 no C7C C8C C9C 118.9(25) 1_555 1_555 1_555 no C8C C9C C10C 120.9(26) 1_555 1_555 1_555 no N2C C10C C9C 123.9(24) 1_555 1_555 1_555 no N2C C11C C7C 126.4(24) 1_555 1_555 1_555 no N2C C11C C12C 113.8(20) 1_555 1_555 1_555 no C7C C11C C12C 119.7(23) 1_555 1_555 1_555 no N1C C12C C4C 124.9(23) 1_555 1_555 1_555 no N1C C12C C11C 114.9(21) 1_555 1_555 1_555 no C4C C12C C11C 120.2(22) 1_555 1_555 1_555 no I1 Hg I2 109.61(7) 1_555 1_555 1_555 no I1 Hg I3 120.07(7) 1_555 1_555 1_555 no I1 Hg I4 97.95(6) 1_555 1_555 1_555 no I2 Hg I3 106.26(8) 1_555 1_555 1_555 no I2 Hg I4 116.38(9) 1_555 1_555 1_555 no I3 Hg I4 106.98(7) 1_555 1_555 1_555 no O1Ac C1Ac C2Ac 118.5(16) 1_555 1_555 1_555 no O1Ac C1Ac C3Ac 118.5(16) 1_555 1_555 1_555 no C2Ac C1Ac C3Ac 123.1(32) 1_555 1_555 1_555 no data_DID258_D-(H2O)1.5 _database_code_CSD 212714 _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C36 H24 Fe N6 2+,Hg I4 2-,1.5(H2 O)' _chemical_formula_sum 'C36 H27 Fe Hg I4 N6 O1.5' _chemical_formula_iupac ? _chemical_formula_weight 1331.7 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 10.180(6) _cell_length_b 17.079(7) _cell_length_c 23.620(8) _cell_angle_alpha 90 _cell_angle_beta 97.22(3) _cell_angle_gamma 90 _cell_volume 4074(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.17 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2460.0 _exptl_absorpt_coefficient_mu 7.154 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.18 _exptl_absorpt_correction_T_max 0.63 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 7356 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 7170 _reflns_number_gt 4071 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.052 _refine_ls_wR_factor_ref 0.058 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4071 _refine_ls_number_parameters 233 _refine_ls_goodness_of_fit_ref 1.63 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.008 _refine_diff_density_max 3.21 _refine_diff_density_min -2.17 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Fe 0.39027(16) 0.25490(10) 0.09932(7) 0.0346(4) Uani Fe 1.0 N1A 0.2234(9) 0.3154(6) 0.0905(4) 0.039(2) Uani N 1.0 N2A 0.3380(10) 0.2349(6) 0.1764(4) 0.041(2) Uani N 1.0 C1A 0.1673(13) 0.3549(8) 0.0464(6) 0.048(2) Uani C 1.0 C2A 0.0470(15) 0.3956(9) 0.0471(7) 0.063(4) Uani C 1.0 C3A -0.0158(15) 0.3932(10) 0.0937(7) 0.070(4) Uani C 1.0 C4A 0.0358(14) 0.3477(10) 0.1403(7) 0.063(3) Uani C 1.0 C5A -0.0270(15) 0.3326(12) 0.1906(8) 0.081(4) Uani C 1.0 C6A 0.0281(17) 0.2891(13) 0.2334(8) 0.085(5) Uani C 1.0 C7A 0.1586(15) 0.2528(10) 0.2308(6) 0.067(3) Uani C 1.0 C8A 0.2196(18) 0.2079(12) 0.2746(7) 0.080(5) Uani C 1.0 C9A 0.3427(16) 0.1786(10) 0.2677(6) 0.071(5) Uani C 1.0 C10A 0.3982(14) 0.1900(8) 0.2174(6) 0.051(3) Uani C 1.0 C11A 0.2183(13) 0.2651(8) 0.1832(6) 0.048(2) Uani C 1.0 C12A 0.1594(12) 0.3110(8) 0.1367(6) 0.046(2) Uani C 1.0 N1B 0.3003(9) 0.1560(6) 0.0746(4) 0.038(2) Uani N 1.0 N2B 0.5475(9) 0.1858(6) 0.1134(4) 0.039(2) Uani N 1.0 C1B 0.1723(12) 0.1411(8) 0.0579(5) 0.044(2) Uani C 1.0 C2B 0.1220(13) 0.0669(9) 0.0477(7) 0.062(3) Uani C 1.0 C3B 0.2051(15) 0.0036(9) 0.0509(8) 0.077(2) Uani C 1.0 C4B 0.3426(15) 0.0176(9) 0.0686(8) 0.071(2) Uani C 1.0 C5B 0.4394(17) -0.0430(10) 0.0748(10) 0.098(3) Uani C 1.0 C6B 0.5633(17) -0.0284(10) 0.0948(10) 0.100(3) Uani C 1.0 C7B 0.6084(15) 0.0501(9) 0.1084(8) 0.073(2) Uani C 1.0 C8B 0.7368(15) 0.0690(9) 0.1320(8) 0.081(4) Uani C 1.0 C9B 0.7680(13) 0.1447(9) 0.1457(7) 0.065(3) Uani C 1.0 C10B 0.6689(12) 0.2026(8) 0.1364(6) 0.046(2) Uani C 1.0 C11B 0.5179(13) 0.1101(8) 0.0994(6) 0.050(2) Uani C 1.0 C12B 0.3834(13) 0.0932(8) 0.0799(6) 0.050(2) Uani C 1.0 N1C 0.4365(9) 0.2821(6) 0.0227(4) 0.037(2) Uani N 1.0 N2C 0.4924(9) 0.3498(6) 0.1214(4) 0.036(2) Uani N 1.0 C1C 0.4052(13) 0.2471(8) -0.0256(5) 0.044(2) Uani C 1.0 C2C 0.4479(15) 0.2713(9) -0.0759(6) 0.055(3) Uani C 1.0 C3C 0.5262(14) 0.3360(9) -0.0755(6) 0.056(3) Uani C 1.0 C4C 0.5636(13) 0.3754(8) -0.0248(6) 0.048(2) Uani C 1.0 C5C 0.6480(13) 0.4449(9) -0.0169(6) 0.054(2) Uani C 1.0 C6C 0.6763(13) 0.4794(8) 0.0333(7) 0.053(2) Uani C 1.0 C7C 0.6260(12) 0.4501(8) 0.0831(6) 0.047(2) Uani C 1.0 C8C 0.6541(13) 0.4833(8) 0.1379(6) 0.055(2) Uani C 1.0 C9C 0.5973(14) 0.4502(8) 0.1810(6) 0.054(2) Uani C 1.0 C10C 0.5175(12) 0.3843(8) 0.1718(5) 0.044(2) Uani C 1.0 C11C 0.5462(11) 0.3839(7) 0.0769(5) 0.039(2) Uani C 1.0 C12C 0.5126(11) 0.3466(7) 0.0234(5) 0.039(1) Uani C 1.0 Hg 0.10934(6) 0.74183(4) 0.60328(3) 0.0551(2) Uani Hg 1.0 I1 0.18534(9) 0.72025(6) 0.49710(4) 0.0533(3) Uani I 1.0 I2 -0.09673(11) 0.63675(7) 0.61195(5) 0.0772(4) Uani I 1.0 I3 0.30744(11) 0.70976(9) 0.69216(5) 0.0902(5) Uani I 1.0 I4 0.01402(16) 0.89232(8) 0.62015(6) 0.1042(5) Uani I 1.0 OW1 0.3464(36) 0.9261(27) 0.7094(19) 0.425(9) Uani O 1.0 OW2 0.0844(96) 0.0243(64) 0.2220(42) 0.283(9) Uani O 0.25 OW2' 0.1878(97) -0.0039(63) 0.1965(41) 0.283(9) Uani O 0.25 HC1A 0.2114 0.3561 0.0109 0.050 Uani H 1.0 HC2A 0.0085 0.4262 0.0129 0.076 Uani H 1.0 HC3A -0.0990 0.4239 0.0951 0.088 Uani H 1.0 HC5A -0.1161 0.3560 0.1931 0.100 Uani H 1.0 HC6A -0.0189 0.2808 0.2677 0.106 Uani H 1.0 HC8A 0.1770 0.1969 0.3096 0.102 Uani H 1.0 HC9A 0.3934 0.1485 0.2995 0.086 Uani H 1.0 HC10A 0.4840 0.1642 0.2122 0.052 Uani H 1.0 HC1B 0.1096 0.1864 0.0525 0.044 Uani H 1.0 HC2B 0.0244 0.0592 0.0379 0.071 Uani H 1.0 HC3B 0.1710 -0.0502 0.0412 0.099 Uani H 1.0 HC5B 0.4125 -0.0978 0.0638 0.124 Uani H 1.0 HC6B 0.6277 -0.0727 0.1007 0.127 Uani H 1.0 HC8B 0.8058 0.0272 0.1387 0.105 Uani H 1.0 HC9B 0.8602 0.1590 0.1621 0.076 Uani H 1.0 HC10B 0.6913 0.2579 0.1476 0.044 Uani H 1.0 HC1C 0.3468 0.1999 -0.0266 0.047 Uani H 1.0 HC2C 0.4218 0.2418 -0.1121 0.067 Uani H 1.0 HC3C 0.5565 0.3551 -0.1118 0.067 Uani H 1.0 HC5C 0.6857 0.4670 -0.0505 0.063 Uani H 1.0 HC6C 0.7340 0.5270 0.0366 0.062 Uani H 1.0 HC8C 0.7138 0.5297 0.1448 0.065 Uani H 1.0 HC9C 0.6132 0.4735 0.2201 0.065 Uani H 1.0 HC10C 0.4771 0.3619 0.2047 0.046 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Fe 0.0318(9) 0.026(1) 0.047(1) 0.0019(8) 0.0084(7) 0.0018(8) Fe N1A 0.036(3) 0.021(3) 0.059(3) 0.001(2) 0.004(2) -0.003(2) N N2A 0.042(2) 0.029(3) 0.052(3) -0.006(2) 0.009(2) 0.002(2) N C1A 0.045(3) 0.026(3) 0.068(3) 0.007(2) -0.003(2) 0.000(2) C C2A 0.052(3) 0.042(5) 0.091(5) 0.018(4) -0.009(3) -0.007(4) C C3A 0.046(3) 0.060(5) 0.102(6) 0.021(3) -0.002(3) -0.023(4) C C4A 0.040(3) 0.063(4) 0.086(4) 0.008(2) 0.010(3) -0.022(3) C C5A 0.046(3) 0.105(7) 0.097(5) 0.004(3) 0.024(4) -0.031(5) C C6A 0.057(4) 0.118(8) 0.085(4) -0.008(4) 0.034(4) -0.021(4) C C7A 0.057(3) 0.083(5) 0.066(3) -0.011(3) 0.025(3) -0.005(3) C C8A 0.080(5) 0.102(8) 0.063(3) -0.016(5) 0.027(3) 0.010(3) C C9A 0.080(5) 0.076(7) 0.058(3) -0.011(4) 0.014(3) 0.018(3) C C10A 0.057(3) 0.041(4) 0.054(3) -0.006(2) 0.007(2) 0.011(2) C C11A 0.042(2) 0.045(3) 0.058(3) -0.006(2) 0.014(2) -0.004(2) C C12A 0.036(3) 0.037(3) 0.065(3) 0.001(2) 0.009(2) -0.010(2) C N1B 0.032(2) 0.031(2) 0.051(4) 0.001(2) 0.007(2) 0.001(2) N N2B 0.030(2) 0.032(2) 0.055(4) 0.003(2) 0.009(2) 0.003(2) N C1B 0.034(2) 0.034(2) 0.064(4) -0.002(2) 0.003(3) 0.002(3) C C2B 0.042(2) 0.036(3) 0.103(7) -0.005(3) -0.007(4) 0.000(4) C C3B 0.051(4) 0.034(2) 0.140(7) -0.003(3) -0.013(5) -0.009(3) C C4B 0.047(3) 0.032(2) 0.130(5) 0.002(2) -0.007(3) -0.010(3) C C5B 0.057(5) 0.033(2) 0.197(9) 0.008(2) -0.015(5) -0.020(3) C C6B 0.054(4) 0.035(2) 0.204(9) 0.012(2) -0.012(5) -0.016(3) C C7B 0.041(2) 0.035(2) 0.141(6) 0.010(2) -0.002(3) -0.006(3) C C8B 0.039(3) 0.040(3) 0.159(8) 0.012(3) -0.005(4) -0.001(4) C C9B 0.033(2) 0.041(3) 0.119(7) 0.007(2) -0.002(3) 0.006(4) C C10B 0.030(2) 0.036(2) 0.071(4) 0.003(2) 0.005(3) 0.006(3) C C11B 0.035(2) 0.032(2) 0.084(4) 0.005(2) 0.005(2) -0.002(2) C C12B 0.037(2) 0.031(2) 0.080(4) 0.003(2) 0.003(2) -0.004(2) C N1C 0.033(3) 0.033(2) 0.046(2) 0.010(2) 0.008(2) 0.003(2) N N2C 0.029(3) 0.029(3) 0.051(2) 0.007(2) 0.004(2) 0.000(2) N C1C 0.047(3) 0.042(3) 0.045(3) 0.009(2) 0.009(2) 0.001(2) C C2C 0.066(5) 0.055(5) 0.047(2) 0.011(3) 0.015(2) 0.004(2) C C3C 0.062(5) 0.055(5) 0.056(2) 0.015(3) 0.023(3) 0.013(2) C C4C 0.043(3) 0.042(3) 0.062(2) 0.013(2) 0.019(3) 0.014(2) C C5C 0.041(4) 0.042(4) 0.082(4) 0.012(3) 0.023(4) 0.020(3) C C6C 0.035(4) 0.036(3) 0.091(5) 0.007(3) 0.016(4) 0.015(3) C C7C 0.032(3) 0.032(3) 0.076(3) 0.005(2) 0.008(3) 0.006(2) C C8C 0.043(4) 0.035(3) 0.085(4) -0.002(3) 0.002(4) -0.002(3) C C9C 0.050(4) 0.038(3) 0.071(3) -0.002(3) -0.001(3) -0.009(3) C C10C 0.041(3) 0.034(3) 0.055(2) 0.004(2) 0.002(2) -0.005(2) C C11C 0.028(3) 0.029(3) 0.059(2) 0.008(2) 0.007(2) 0.004(2) C C12C 0.032(3) 0.033(2) 0.053(2) 0.011(2) 0.011(2) 0.007(2) C Hg 0.0483(3) 0.0491(4) 0.0690(4) -0.0036(3) 0.0121(3) 0.0060(3) Hg I1 0.0442(5) 0.0474(6) 0.0699(6) -0.0055(4) 0.0140(4) 0.0011(5) I I2 0.0540(7) 0.0780(9) 0.1008(9) -0.0278(6) 0.0148(6) 0.0010(7) I I3 0.0505(7) 0.139(1) 0.0788(8) -0.0074(7) 0.0009(5) 0.0285(8) I I4 0.151(1) 0.0516(8) 0.122(1) 0.0290(8) 0.062(1) 0.0167(7) I OW1 0.305(9) 0.457(9) 0.534(9) -0.127(9) 0.138(9) 0.086(9) O OW2 0.283(9) 0.283(9) 0.283(9) 0.0000(0) 0.036(5) 0.0000(0) O OW2' 0.283(9) 0.283(9) 0.283(9) 0.0000(0) 0.036(5) 0.0000(0) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1A 1.977(10) 1_555 1_555 no Fe N2A 1.989(10) 1_555 1_555 no Fe N1B 1.975(10) 1_555 1_555 no Fe N2B 1.983(10) 1_555 1_555 no Fe N1C 1.982(9) 1_555 1_555 no Fe N2C 1.961(10) 1_555 1_555 no N1A C1A 1.311(15) 1_555 1_555 no N1A C12A 1.340(15) 1_555 1_555 no N2A C10A 1.325(16) 1_555 1_555 no N2A C11A 1.351(16) 1_555 1_555 no C1A C2A 1.410(18) 1_555 1_555 no C2A C3A 1.342(21) 1_555 1_555 no C3A C4A 1.395(21) 1_555 1_555 no C4A C5A 1.440(21) 1_555 1_555 no C4A C12A 1.418(18) 1_555 1_555 no C5A C6A 1.322(24) 1_555 1_555 no C6A C7A 1.475(22) 1_555 1_555 no C7A C8A 1.372(22) 1_555 1_555 no C7A C11A 1.359(18) 1_555 1_555 no C8A C9A 1.378(22) 1_555 1_555 no C9A C10A 1.391(18) 1_555 1_555 no C11A C12A 1.421(18) 1_555 1_555 no N1B C1B 1.338(14) 1_555 1_555 no N1B C12B 1.361(15) 1_555 1_555 no N2B C10B 1.318(15) 1_555 1_555 no N2B C11B 1.359(16) 1_555 1_555 no C1B C2B 1.376(19) 1_555 1_555 no C2B C3B 1.369(20) 1_555 1_555 no C3B C4B 1.429(20) 1_555 1_555 no C4B C5B 1.424(21) 1_555 1_555 no C4B C12B 1.373(19) 1_555 1_555 no C5B C6B 1.315(22) 1_555 1_555 no C6B C7B 1.440(22) 1_555 1_555 no C7B C8B 1.393(20) 1_555 1_555 no C7B C11B 1.376(19) 1_555 1_555 no C8B C9B 1.359(21) 1_555 1_555 no C9B C10B 1.411(18) 1_555 1_555 no C11B C12B 1.418(17) 1_555 1_555 no N1C C1C 1.292(15) 1_555 1_555 no N1C C12C 1.345(15) 1_555 1_555 no N2C C10C 1.325(15) 1_555 1_555 no N2C C11C 1.374(15) 1_555 1_555 no C1C C2C 1.378(18) 1_555 1_555 no C2C C3C 1.362(20) 1_555 1_555 no C3C C4C 1.386(19) 1_555 1_555 no C4C C5C 1.463(19) 1_555 1_555 no C4C C12C 1.399(17) 1_555 1_555 no C5C C6C 1.323(19) 1_555 1_555 no C6C C7C 1.430(18) 1_555 1_555 no C7C C8C 1.409(18) 1_555 1_555 no C7C C11C 1.390(17) 1_555 1_555 no C8C C9C 1.356(19) 1_555 1_555 no C9C C10C 1.389(18) 1_555 1_555 no C11C C12C 1.416(17) 1_555 1_555 no Hg I1 2.741(1) 1_555 1_555 no Hg I2 2.788(1) 1_555 1_555 no Hg I3 2.777(1) 1_555 1_555 no Hg I4 2.793(1) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Fe N2A 82.0(4) 1_555 1_555 1_555 no N1A Fe N1B 93.2(4) 1_555 1_555 1_555 no N1A Fe N2B 173.5(4) 1_555 1_555 1_555 no N1A Fe N1C 94.7(4) 1_555 1_555 1_555 no N1A Fe N2C 90.9(4) 1_555 1_555 1_555 no N2A Fe N1B 87.5(4) 1_555 1_555 1_555 no N2A Fe N2B 92.7(4) 1_555 1_555 1_555 no N2A Fe N1C 176.0(4) 1_555 1_555 1_555 no N2A Fe N2C 95.3(4) 1_555 1_555 1_555 no N1B Fe N2B 82.8(4) 1_555 1_555 1_555 no N1B Fe N1C 94.9(4) 1_555 1_555 1_555 no N1B Fe N2C 175.3(4) 1_555 1_555 1_555 no N2B Fe N1C 90.8(4) 1_555 1_555 1_555 no N2B Fe N2C 93.3(4) 1_555 1_555 1_555 no N1C Fe N2C 82.5(4) 1_555 1_555 1_555 no Fe N1A C1A 129.4(9) 1_555 1_555 1_555 no Fe N1A C12A 112.6(8) 1_555 1_555 1_555 no C1A N1A C12A 117.9(11) 1_555 1_555 1_555 no Fe N2A C10A 128.1(9) 1_555 1_555 1_555 no Fe N2A C11A 113.2(8) 1_555 1_555 1_555 no C10A N2A C11A 118.3(11) 1_555 1_555 1_555 no N1A C1A C2A 122.4(13) 1_555 1_555 1_555 no C1A C2A C3A 119.9(14) 1_555 1_555 1_555 no C2A C3A C4A 119.6(13) 1_555 1_555 1_555 no C3A C4A C5A 126.0(14) 1_555 1_555 1_555 no C3A C4A C12A 116.5(14) 1_555 1_555 1_555 no C5A C4A C12A 117.4(15) 1_555 1_555 1_555 no C4A C5A C6A 122.8(15) 1_555 1_555 1_555 no C5A C6A C7A 120.1(14) 1_555 1_555 1_555 no C6A C7A C8A 121.9(14) 1_555 1_555 1_555 no C6A C7A C11A 118.0(15) 1_555 1_555 1_555 no C8A C7A C11A 120.1(15) 1_555 1_555 1_555 no C7A C8A C9A 116.5(14) 1_555 1_555 1_555 no C8A C9A C10A 121.6(15) 1_555 1_555 1_555 no N2A C10A C9A 120.3(13) 1_555 1_555 1_555 no N2A C11A C7A 123.0(13) 1_555 1_555 1_555 no N2A C11A C12A 114.7(11) 1_555 1_555 1_555 no C7A C11A C12A 122.4(13) 1_555 1_555 1_555 no N1A C12A C4A 123.4(13) 1_555 1_555 1_555 no N1A C12A C11A 117.3(11) 1_555 1_555 1_555 no C4A C12A C11A 119.2(13) 1_555 1_555 1_555 no Fe N1B C1B 130.4(9) 1_555 1_555 1_555 no Fe N1B C12B 112.7(8) 1_555 1_555 1_555 no C1B N1B C12B 116.7(11) 1_555 1_555 1_555 no Fe N2B C10B 129.4(9) 1_555 1_555 1_555 no Fe N2B C11B 112.1(8) 1_555 1_555 1_555 no C10B N2B C11B 118.4(11) 1_555 1_555 1_555 no N1B C1B C2B 123.6(12) 1_555 1_555 1_555 no C1B C2B C3B 120.2(13) 1_555 1_555 1_555 no C2B C3B C4B 117.4(14) 1_555 1_555 1_555 no C3B C4B C5B 123.3(14) 1_555 1_555 1_555 no C3B C4B C12B 118.4(13) 1_555 1_555 1_555 no C5B C4B C12B 118.4(14) 1_555 1_555 1_555 no C4B C5B C6B 121.3(15) 1_555 1_555 1_555 no C5B C6B C7B 121.5(15) 1_555 1_555 1_555 no C6B C7B C8B 124.2(14) 1_555 1_555 1_555 no C6B C7B C11B 118.0(14) 1_555 1_555 1_555 no C8B C7B C11B 117.8(14) 1_555 1_555 1_555 no C7B C8B C9B 119.7(14) 1_555 1_555 1_555 no C8B C9B C10B 119.2(13) 1_555 1_555 1_555 no N2B C10B C9B 121.8(13) 1_555 1_555 1_555 no N2B C11B C7B 123.2(13) 1_555 1_555 1_555 no N2B C11B C12B 116.6(11) 1_555 1_555 1_555 no C7B C11B C12B 120.0(13) 1_555 1_555 1_555 no N1B C12B C4B 123.6(12) 1_555 1_555 1_555 no N1B C12B C11B 115.7(12) 1_555 1_555 1_555 no C4B C12B C11B 120.7(13) 1_555 1_555 1_555 no Fe N1C C1C 129.6(9) 1_555 1_555 1_555 no Fe N1C C12C 112.5(8) 1_555 1_555 1_555 no C1C N1C C12C 117.9(11) 1_555 1_555 1_555 no Fe N2C C10C 130.0(9) 1_555 1_555 1_555 no Fe N2C C11C 113.3(8) 1_555 1_555 1_555 no C10C N2C C11C 116.7(11) 1_555 1_555 1_555 no N1C C1C C2C 123.5(13) 1_555 1_555 1_555 no C1C C2C C3C 119.1(13) 1_555 1_555 1_555 no C2C C3C C4C 119.7(12) 1_555 1_555 1_555 no C3C C4C C5C 126.7(12) 1_555 1_555 1_555 no C3C C4C C12C 116.3(13) 1_555 1_555 1_555 no C5C C4C C12C 117.0(13) 1_555 1_555 1_555 no C4C C5C C6C 122.3(13) 1_555 1_555 1_555 no C5C C6C C7C 121.3(14) 1_555 1_555 1_555 no C6C C7C C8C 124.2(13) 1_555 1_555 1_555 no C6C C7C C11C 117.6(13) 1_555 1_555 1_555 no C8C C7C C11C 118.2(12) 1_555 1_555 1_555 no C7C C8C C9C 117.8(13) 1_555 1_555 1_555 no C8C C9C C10C 121.1(13) 1_555 1_555 1_555 no N2C C10C C9C 123.0(12) 1_555 1_555 1_555 no N2C C11C C7C 123.2(12) 1_555 1_555 1_555 no N2C C11C C12C 114.6(11) 1_555 1_555 1_555 no C7C C11C C12C 122.2(12) 1_555 1_555 1_555 no N1C C12C C4C 123.3(12) 1_555 1_555 1_555 no N1C C12C C11C 117.0(11) 1_555 1_555 1_555 no C4C C12C C11C 119.6(12) 1_555 1_555 1_555 no I1 Hg I2 106.39(4) 1_555 1_555 1_555 no I1 Hg I3 113.80(4) 1_555 1_555 1_555 no I1 Hg I4 113.41(4) 1_555 1_555 1_555 no I2 Hg I3 107.41(4) 1_555 1_555 1_555 no I2 Hg I4 107.68(5) 1_555 1_555 1_555 no I3 Hg I4 107.81(5) 1_555 1_555 1_555 no data_DID279_E-(dmf)2 _database_code_CSD 212715 _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C36 H24 Fe N6 2+,Hg I4 2-,2(C3 H7 N O)' _chemical_formula_sum 'C42 H38 Fe Hg I4 N8 O2' _chemical_formula_iupac ? _chemical_formula_weight 1450.9 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 19.180(6) _cell_length_b 19.465(3) _cell_length_c 13.492(4) _cell_angle_alpha 90 _cell_angle_beta 109.44(1) _cell_angle_gamma 90 _cell_volume 4750(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.03 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720.0 _exptl_absorpt_coefficient_mu 6.147 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.66 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 6798 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_theta_max 23 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 6576 _reflns_number_gt 3531 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.035 _refine_ls_wR_factor_ref 0.042 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3531 _refine_ls_number_parameters 257 _refine_ls_goodness_of_fit_ref 1.30 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.008 _refine_diff_density_max 1.80 _refine_diff_density_min -1.90 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Fe 0.26148(7) 0.56659(7) 0.51730(10) 0.0350(4) Uani Fe 1.0 N1A 0.2603(4) 0.6693(4) 0.5159(6) 0.037(1) Uani N 1.0 N2A 0.2121(4) 0.5796(4) 0.6230(6) 0.037(1) Uani N 1.0 C1A 0.2871(6) 0.7138(5) 0.4614(8) 0.043(1) Uani C 1.0 C2A 0.2800(6) 0.7838(5) 0.4693(8) 0.052(1) Uani C 1.0 C3A 0.2447(6) 0.8101(5) 0.5321(9) 0.054(1) Uani C 1.0 C4A 0.2170(6) 0.7656(5) 0.5920(8) 0.048(1) Uani C 1.0 C5A 0.1776(6) 0.7870(6) 0.6598(9) 0.056(2) Uani C 1.0 C6A 0.1524(6) 0.7413(6) 0.7138(9) 0.057(2) Uani C 1.0 C7A 0.1625(6) 0.6691(6) 0.7038(8) 0.049(2) Uani C 1.0 C8A 0.1383(6) 0.6188(6) 0.7610(8) 0.057(2) Uani C 1.0 C9A 0.1506(6) 0.5513(6) 0.7454(8) 0.054(2) Uani C 1.0 C10A 0.1887(6) 0.5337(5) 0.6748(8) 0.043(1) Uani C 1.0 C11A 0.1990(5) 0.6475(5) 0.6370(7) 0.040(1) Uani C 1.0 C12A 0.2271(5) 0.6959(5) 0.5813(7) 0.040(1) Uani C 1.0 N1B 0.1642(4) 0.5592(4) 0.4073(6) 0.039(1) Uani N 1.0 N2B 0.2547(4) 0.4655(4) 0.5128(6) 0.040(1) Uani N 1.0 C1B 0.1163(6) 0.6077(6) 0.3609(8) 0.047(1) Uani C 1.0 C2B 0.0499(6) 0.5931(7) 0.2796(9) 0.060(2) Uani C 1.0 C3B 0.0346(6) 0.5284(7) 0.2457(9) 0.065(2) Uani C 1.0 C4B 0.0823(6) 0.4753(6) 0.2942(9) 0.058(1) Uani C 1.0 C5B 0.0717(7) 0.4048(7) 0.2641(10) 0.074(2) Uani C 1.0 C6B 0.1193(7) 0.3562(7) 0.3155(10) 0.077(2) Uani C 1.0 C7B 0.1846(7) 0.3738(6) 0.4037(9) 0.063(2) Uani C 1.0 C8B 0.2353(8) 0.3259(6) 0.4670(11) 0.074(3) Uani C 1.0 C9B 0.2923(7) 0.3476(6) 0.5487(10) 0.067(3) Uani C 1.0 C10B 0.3004(6) 0.4187(5) 0.5708(9) 0.050(2) Uani C 1.0 C11B 0.1964(6) 0.4414(5) 0.4315(8) 0.046(1) Uani C 1.0 C12B 0.1465(6) 0.4924(5) 0.3751(8) 0.045(1) Uani C 1.0 N1C 0.3154(4) 0.5635(4) 0.4156(6) 0.039(2) Uani N 1.0 N2C 0.3625(4) 0.5688(4) 0.6213(6) 0.039(2) Uani N 1.0 C1C 0.2923(6) 0.5574(5) 0.3125(8) 0.045(2) Uani C 1.0 C2C 0.3377(6) 0.5626(6) 0.2522(8) 0.053(2) Uani C 1.0 C3C 0.4102(6) 0.5764(6) 0.2974(8) 0.054(2) Uani C 1.0 C4C 0.4398(6) 0.5824(5) 0.4072(8) 0.048(2) Uani C 1.0 C5C 0.5159(6) 0.5926(6) 0.4677(9) 0.054(2) Uani C 1.0 C6C 0.5412(6) 0.5927(6) 0.5734(9) 0.056(2) Uani C 1.0 C7C 0.4910(6) 0.5840(5) 0.6316(8) 0.050(2) Uani C 1.0 C8C 0.5121(6) 0.5807(6) 0.7404(8) 0.057(3) Uani C 1.0 C9C 0.4593(6) 0.5715(6) 0.7869(8) 0.056(3) Uani C 1.0 C10C 0.3852(6) 0.5653(5) 0.7263(7) 0.046(2) Uani C 1.0 C11C 0.4162(5) 0.5759(5) 0.5755(7) 0.042(1) Uani C 1.0 C12C 0.3896(6) 0.5745(5) 0.4630(8) 0.041(2) Uani C 1.0 Hg 0.23802(3) 0.42885(2) 0.00121(4) 0.0562(2) Uani Hg 1.0 I1 0.12917(4) 0.51597(4) 0.03003(6) 0.0579(2) Uani I 1.0 I2 0.35297(5) 0.51164(4) -0.01736(6) 0.0633(3) Uani I 1.0 I3 0.28076(5) 0.34240(5) 0.17282(6) 0.0748(3) Uani I 1.0 I4 0.18249(5) 0.35757(4) -0.18792(6) 0.0708(3) Uani I 1.0 O1D1 -0.0553(5) 0.2431(5) 0.6192(7) 0.111(4) Uani O 1.0 N1D1 0.0201(4) 0.2388(5) 0.5277(5) 0.089(4) Uani N 1.0 C1D1 -0.0262(6) 0.2107(5) 0.5663(8) 0.103(5) Uani C 1.0 C2D1 0.0428(11) 0.3059(8) 0.5391(15) 0.192(9) Uani C 1.0 C3D1 0.0510(9) 0.1958(8) 0.4666(12) 0.157(8) Uani C 1.0 O1D2 0.4438(6) 0.1269(7) 0.2606(8) 0.194(6) Uani O 1.0 N1D2 0.4488(6) 0.1882(4) 0.3993(7) 0.098(5) Uani N 1.0 C1D2 0.4148(6) 0.1479(7) 0.3226(11) 0.175(6) Uani C 1.0 C2D2 0.5193(10) 0.2129(11) 0.4224(17) 0.232(9) Uani C 1.0 C3D2 0.4093(9) 0.2097(8) 0.4674(12) 0.136(6) Uani C 1.0 HC1A 0.3129 0.6955 0.4136 0.045 Uani H 1.0 HC2A 0.3011 0.8154 0.4281 0.062 Uani H 1.0 HC3A 0.2383 0.8609 0.5359 0.064 Uani H 1.0 HC5A 0.1686 0.8371 0.6670 0.065 Uani H 1.0 HC6A 0.1260 0.7579 0.7619 0.067 Uani H 1.0 HC8A 0.1128 0.6325 0.8116 0.068 Uani H 1.0 HC9A 0.1330 0.5145 0.7832 0.064 Uani H 1.0 HC10A 0.1980 0.4841 0.6644 0.045 Uani H 1.0 HC1B 0.1277 0.6564 0.3844 0.049 Uani H 1.0 HC2B 0.0143 0.6309 0.2472 0.072 Uani H 1.0 HC3B -0.0113 0.5182 0.1854 0.080 Uani H 1.0 HC5B 0.0276 0.3914 0.2029 0.090 Uani H 1.0 HC6B 0.1098 0.3071 0.2929 0.095 Uani H 1.0 HC8B 0.2285 0.2757 0.4508 0.093 Uani H 1.0 HC9B 0.3287 0.3140 0.5936 0.081 Uani H 1.0 HC10B 0.3426 0.4343 0.6330 0.051 Uani H 1.0 HC1C 0.2385 0.5484 0.2757 0.047 Uani H 1.0 HC2C 0.3166 0.5562 0.1744 0.062 Uani H 1.0 HC3C 0.4426 0.5823 0.2532 0.063 Uani H 1.0 HC5C 0.5520 0.6001 0.4296 0.062 Uani H 1.0 HC6C 0.5952 0.5988 0.6119 0.064 Uani H 1.0 HC8C 0.5654 0.5849 0.7844 0.067 Uani H 1.0 HC9C 0.4742 0.5693 0.8653 0.065 Uani H 1.0 HC10C 0.3478 0.5580 0.7622 0.047 Uani H 1.0 HC1D1 -0.0384 0.1609 0.5524 0.212 Uani H 1.0 H1C2D1 0.0179 0.3309 0.5828 0.315 Uani H 1.0 H2C2D1 0.0976 0.3078 0.5745 0.271 Uani H 1.0 H3C2D1 0.0295 0.3281 0.4684 0.257 Uani H 1.0 H1C3D1 0.0307 0.1482 0.4636 0.320 Uani H 1.0 H2C3D1 0.0380 0.2147 0.3938 0.187 Uani H 1.0 H3C3D1 0.1060 0.1944 0.4999 0.197 Uani H 1.0 HC1D2 0.3630 0.1333 0.3138 0.368 Uani H 1.0 H1C2D2 0.5414 0.1947 0.3702 0.285 Uani H 1.0 H2C2D2 0.5182 0.2642 0.4194 0.380 Uani H 1.0 H3C2D2 0.5499 0.1977 0.4946 0.375 Uani H 1.0 H1C3D2 0.3588 0.1887 0.4432 0.270 Uani H 1.0 H2C3D2 0.4366 0.1944 0.5408 0.247 Uani H 1.0 H3C3D2 0.4049 0.2609 0.4656 0.144 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Fe 0.0370(8) 0.0344(8) 0.0357(8) -0.0008(7) 0.0149(7) -0.0022(7) Fe N1A 0.037(2) 0.034(2) 0.037(2) -0.003(2) 0.009(2) 0.001(2) N N2A 0.035(3) 0.040(2) 0.036(2) -0.002(2) 0.012(2) 0.001(2) N C1A 0.048(3) 0.036(2) 0.044(2) -0.005(2) 0.014(2) 0.003(2) C C2A 0.066(4) 0.035(2) 0.055(4) -0.006(2) 0.019(3) 0.003(2) C C3A 0.070(5) 0.035(2) 0.056(4) 0.000(2) 0.016(3) 0.000(2) C C4A 0.056(3) 0.038(2) 0.047(3) 0.004(2) 0.013(2) -0.003(2) C C5A 0.067(4) 0.047(2) 0.054(4) 0.011(3) 0.018(3) -0.007(2) C C6A 0.064(4) 0.056(2) 0.053(3) 0.013(3) 0.023(3) -0.007(3) C C7A 0.052(3) 0.053(2) 0.047(2) 0.006(2) 0.021(2) -0.003(2) C C8A 0.062(4) 0.065(3) 0.054(3) 0.004(3) 0.033(3) -0.001(3) C C9A 0.060(4) 0.060(3) 0.053(3) -0.002(3) 0.032(3) 0.003(3) C C10A 0.045(3) 0.046(2) 0.043(2) -0.004(2) 0.020(2) 0.003(2) C C11A 0.040(2) 0.042(2) 0.038(2) 0.002(2) 0.013(2) -0.001(2) C C12A 0.041(2) 0.037(2) 0.039(2) 0.001(2) 0.010(2) -0.001(2) C N1B 0.039(3) 0.046(2) 0.038(3) -0.003(2) 0.022(2) -0.003(2) N N2B 0.046(2) 0.037(2) 0.046(2) -0.002(2) 0.026(2) -0.004(2) N C1B 0.041(3) 0.056(2) 0.046(3) 0.002(2) 0.020(2) 0.003(2) C C2B 0.044(3) 0.079(4) 0.054(3) 0.000(2) 0.013(2) 0.005(3) C C3B 0.049(3) 0.088(4) 0.054(3) -0.012(3) 0.011(2) -0.005(3) C C4B 0.052(3) 0.070(3) 0.052(3) -0.016(2) 0.018(2) -0.014(2) C C5B 0.072(4) 0.077(3) 0.071(4) -0.028(3) 0.021(2) -0.027(3) C C6B 0.084(4) 0.061(2) 0.086(4) -0.026(3) 0.029(3) -0.030(3) C C7B 0.073(3) 0.044(2) 0.076(3) -0.013(2) 0.032(2) -0.018(2) C C8B 0.088(5) 0.038(2) 0.100(6) -0.006(2) 0.038(3) -0.012(2) C C9B 0.078(5) 0.038(2) 0.092(5) 0.004(2) 0.035(3) 0.001(2) C C10B 0.056(3) 0.039(2) 0.061(3) 0.003(2) 0.029(2) 0.002(2) C C11B 0.052(2) 0.041(2) 0.052(2) -0.008(2) 0.027(2) -0.010(2) C C12B 0.045(2) 0.050(2) 0.044(2) -0.009(2) 0.022(2) -0.009(2) C N1C 0.047(2) 0.037(3) 0.037(2) 0.000(2) 0.020(1) -0.001(2) N N2C 0.045(2) 0.038(3) 0.037(2) 0.000(2) 0.017(2) 0.000(2) N C1C 0.053(2) 0.050(3) 0.037(2) -0.001(2) 0.022(2) -0.003(2) C C2C 0.060(3) 0.067(5) 0.041(2) -0.002(3) 0.028(2) -0.003(3) C C3C 0.058(2) 0.067(4) 0.048(2) -0.001(3) 0.031(2) 0.000(3) C C4C 0.050(2) 0.054(3) 0.048(2) 0.000(2) 0.027(2) 0.001(2) C C5C 0.049(2) 0.064(4) 0.058(3) -0.001(2) 0.028(2) 0.003(4) C C6C 0.045(2) 0.068(4) 0.058(3) -0.002(2) 0.022(2) 0.003(4) C C7C 0.045(2) 0.058(3) 0.048(2) -0.002(2) 0.017(2) 0.002(2) C C8C 0.047(2) 0.075(5) 0.047(2) -0.004(2) 0.013(2) 0.003(3) C C9C 0.050(2) 0.074(5) 0.041(2) -0.004(3) 0.012(2) 0.002(3) C C10C 0.048(2) 0.053(3) 0.037(2) -0.002(2) 0.015(2) 0.001(2) C C11C 0.045(2) 0.042(2) 0.041(2) 0.000(2) 0.018(1) 0.001(2) C C12C 0.047(2) 0.040(2) 0.041(2) 0.000(2) 0.022(1) 0.000(2) C Hg 0.0614(3) 0.0546(3) 0.0539(3) -0.0024(3) 0.0210(2) -0.0009(3) Hg I1 0.0571(5) 0.0610(5) 0.0572(5) -0.0003(4) 0.0213(4) -0.0067(4) I I2 0.0668(6) 0.0769(6) 0.0547(5) -0.0117(5) 0.0314(4) 0.0001(4) I I3 0.0813(7) 0.0762(7) 0.0603(5) -0.0066(5) 0.0144(5) 0.0160(5) I I4 0.1043(7) 0.0475(5) 0.0549(5) -0.0059(5) 0.0190(5) -0.0028(4) I O1D1 0.120(7) 0.119(7) 0.105(7) 0.017(6) 0.052(5) 0.010(6) O N1D1 0.081(7) 0.116(6) 0.061(6) 0.011(5) 0.011(5) 0.003(5) N C1D1 0.102(7) 0.119(6) 0.089(7) 0.006(5) 0.035(5) -0.001(5) C C2D1 0.264(9) 0.136(7) 0.262(9) -0.050(7) 0.200(9) -0.060(6) C C3D1 0.208(9) 0.124(6) 0.195(9) -0.016(6) 0.141(9) -0.026(7) C O1D2 0.120(7) 0.291(9) 0.165(9) 0.021(9) 0.039(7) -0.110(9) O N1D2 0.104(7) 0.102(8) 0.103(7) -0.009(6) 0.052(6) -0.003(6) N C1D2 0.105(7) 0.229(9) 0.200(9) -0.020(6) 0.062(6) -0.114(8) C C2D2 0.144(8) 0.268(9) 0.335(9) -0.091(9) 0.149(8) -0.196(9) C C3D2 0.142(7) 0.147(9) 0.151(9) -0.026(6) 0.093(7) -0.034(8) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1A 1.999(8) 1_555 1_555 no Fe N2A 1.973(8) 1_555 1_555 no Fe N1B 1.965(8) 1_555 1_555 no Fe N2B 1.971(8) 1_555 1_555 no Fe N1C 1.975(7) 1_555 1_555 no Fe N2C 1.979(8) 1_555 1_555 no N1A C1A 1.344(12) 1_555 1_555 no N1A C12A 1.352(11) 1_555 1_555 no N2A C10A 1.303(11) 1_555 1_555 no N2A C11A 1.370(12) 1_555 1_555 no C1A C2A 1.377(13) 1_555 1_555 no C2A C3A 1.349(15) 1_555 1_555 no C3A C4A 1.403(14) 1_555 1_555 no C4A C5A 1.429(14) 1_555 1_555 no C4A C12A 1.385(13) 1_555 1_555 no C5A C6A 1.338(15) 1_555 1_555 no C6A C7A 1.432(14) 1_555 1_555 no C7A C8A 1.418(14) 1_555 1_555 no C7A C11A 1.377(13) 1_555 1_555 no C8A C9A 1.363(14) 1_555 1_555 no C9A C10A 1.423(14) 1_555 1_555 no C11A C12A 1.419(13) 1_555 1_555 no N1B C1B 1.320(12) 1_555 1_555 no N1B C12B 1.378(12) 1_555 1_555 no N2B C10B 1.325(12) 1_555 1_555 no N2B C11B 1.362(12) 1_555 1_555 no C1B C2B 1.406(13) 1_555 1_555 no C2B C3B 1.338(16) 1_555 1_555 no C3B C4B 1.393(15) 1_555 1_555 no C4B C5B 1.426(16) 1_555 1_555 no C4B C12B 1.387(14) 1_555 1_555 no C5B C6B 1.337(17) 1_555 1_555 no C6B C7B 1.453(15) 1_555 1_555 no C7B C8B 1.410(16) 1_555 1_555 no C7B C11B 1.368(14) 1_555 1_555 no C8B C9B 1.337(16) 1_555 1_555 no C9B C10B 1.412(14) 1_555 1_555 no C11B C12B 1.412(14) 1_555 1_555 no N1C C1C 1.317(11) 1_555 1_555 no N1C C12C 1.370(11) 1_555 1_555 no N2C C10C 1.338(11) 1_555 1_555 no N2C C11C 1.373(12) 1_555 1_555 no C1C C2C 1.380(13) 1_555 1_555 no C2C C3C 1.347(14) 1_555 1_555 no C3C C4C 1.404(13) 1_555 1_555 no C4C C5C 1.430(14) 1_555 1_555 no C4C C12C 1.414(13) 1_555 1_555 no C5C C6C 1.345(14) 1_555 1_555 no C6C C7C 1.441(14) 1_555 1_555 no C7C C8C 1.388(14) 1_555 1_555 no C7C C11C 1.390(13) 1_555 1_555 no C8C C9C 1.369(14) 1_555 1_555 no C9C C10C 1.389(13) 1_555 1_555 no C11C C12C 1.432(13) 1_555 1_555 no Hg I1 2.815(1) 1_555 1_555 no Hg I2 2.808(1) 1_555 1_555 no Hg I3 2.757(1) 1_555 1_555 no Hg I4 2.786(1) 1_555 1_555 no O1D1 C1D1 1.219(11) 1_555 1_555 no N1D1 C1D1 1.290(13) 1_555 1_555 no N1D1 C2D1 1.369(14) 1_555 1_555 no N1D1 C3D1 1.435(13) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Fe N2A 82.6(3) 1_555 1_555 1_555 no N1A Fe N1B 93.5(3) 1_555 1_555 1_555 no N1A Fe N2B 175.8(3) 1_555 1_555 1_555 no N1A Fe N1C 91.7(3) 1_555 1_555 1_555 no N1A Fe N2C 89.4(3) 1_555 1_555 1_555 no N2A Fe N1B 89.6(3) 1_555 1_555 1_555 no N2A Fe N2B 96.2(3) 1_555 1_555 1_555 no N2A Fe N1C 173.8(3) 1_555 1_555 1_555 no N2A Fe N2C 94.4(3) 1_555 1_555 1_555 no N1B Fe N2B 82.4(3) 1_555 1_555 1_555 no N1B Fe N1C 93.3(3) 1_555 1_555 1_555 no N1B Fe N2C 175.4(3) 1_555 1_555 1_555 no N2B Fe N1C 89.6(3) 1_555 1_555 1_555 no N2B Fe N2C 94.7(3) 1_555 1_555 1_555 no N1C Fe N2C 83.0(3) 1_555 1_555 1_555 no Fe N1A C1A 130.1(7) 1_555 1_555 1_555 no Fe N1A C12A 112.6(6) 1_555 1_555 1_555 no C1A N1A C12A 117.3(9) 1_555 1_555 1_555 no Fe N2A C10A 129.2(7) 1_555 1_555 1_555 no Fe N2A C11A 112.2(6) 1_555 1_555 1_555 no C10A N2A C11A 118.5(9) 1_555 1_555 1_555 no N1A C1A C2A 122.0(10) 1_555 1_555 1_555 no C1A C2A C3A 120.4(11) 1_555 1_555 1_555 no C2A C3A C4A 119.6(10) 1_555 1_555 1_555 no C3A C4A C5A 124.9(10) 1_555 1_555 1_555 no C3A C4A C12A 116.8(10) 1_555 1_555 1_555 no C5A C4A C12A 118.3(10) 1_555 1_555 1_555 no C4A C5A C6A 121.2(10) 1_555 1_555 1_555 no C5A C6A C7A 121.1(10) 1_555 1_555 1_555 no C6A C7A C8A 123.2(10) 1_555 1_555 1_555 no C6A C7A C11A 118.4(10) 1_555 1_555 1_555 no C8A C7A C11A 118.4(10) 1_555 1_555 1_555 no C7A C8A C9A 118.5(10) 1_555 1_555 1_555 no C8A C9A C10A 119.2(10) 1_555 1_555 1_555 no N2A C10A C9A 122.7(10) 1_555 1_555 1_555 no N2A C11A C7A 122.7(10) 1_555 1_555 1_555 no N2A C11A C12A 116.6(9) 1_555 1_555 1_555 no C7A C11A C12A 120.6(10) 1_555 1_555 1_555 no N1A C12A C4A 123.8(10) 1_555 1_555 1_555 no N1A C12A C11A 115.8(9) 1_555 1_555 1_555 no C4A C12A C11A 120.3(10) 1_555 1_555 1_555 no Fe N1B C1B 129.9(7) 1_555 1_555 1_555 no Fe N1B C12B 112.3(7) 1_555 1_555 1_555 no C1B N1B C12B 117.8(9) 1_555 1_555 1_555 no Fe N2B C10B 130.2(7) 1_555 1_555 1_555 no Fe N2B C11B 113.3(7) 1_555 1_555 1_555 no C10B N2B C11B 116.3(9) 1_555 1_555 1_555 no N1B C1B C2B 122.1(10) 1_555 1_555 1_555 no C1B C2B C3B 119.7(11) 1_555 1_555 1_555 no C2B C3B C4B 120.2(11) 1_555 1_555 1_555 no C3B C4B C5B 124.8(11) 1_555 1_555 1_555 no C3B C4B C12B 117.7(11) 1_555 1_555 1_555 no C5B C4B C12B 117.4(11) 1_555 1_555 1_555 no C4B C5B C6B 121.7(11) 1_555 1_555 1_555 no C5B C6B C7B 120.7(11) 1_555 1_555 1_555 no C6B C7B C8B 124.9(11) 1_555 1_555 1_555 no C6B C7B C11B 118.1(11) 1_555 1_555 1_555 no C8B C7B C11B 116.9(11) 1_555 1_555 1_555 no C7B C8B C9B 120.0(11) 1_555 1_555 1_555 no C8B C9B C10B 119.1(12) 1_555 1_555 1_555 no N2B C10B C9B 123.0(11) 1_555 1_555 1_555 no N2B C11B C7B 124.7(11) 1_555 1_555 1_555 no N2B C11B C12B 114.8(9) 1_555 1_555 1_555 no C7B C11B C12B 120.5(11) 1_555 1_555 1_555 no N1B C12B C4B 122.4(10) 1_555 1_555 1_555 no N1B C12B C11B 116.2(9) 1_555 1_555 1_555 no C4B C12B C11B 121.4(10) 1_555 1_555 1_555 no Fe N1C C1C 131.8(7) 1_555 1_555 1_555 no Fe N1C C12C 112.0(6) 1_555 1_555 1_555 no C1C N1C C12C 116.1(8) 1_555 1_555 1_555 no Fe N2C C10C 130.3(7) 1_555 1_555 1_555 no Fe N2C C11C 112.8(6) 1_555 1_555 1_555 no C10C N2C C11C 117.0(8) 1_555 1_555 1_555 no N1C C1C C2C 124.0(10) 1_555 1_555 1_555 no C1C C2C C3C 120.5(10) 1_555 1_555 1_555 no C2C C3C C4C 119.2(10) 1_555 1_555 1_555 no C3C C4C C5C 126.2(10) 1_555 1_555 1_555 no C3C C4C C12C 116.5(10) 1_555 1_555 1_555 no C5C C4C C12C 117.3(9) 1_555 1_555 1_555 no C4C C5C C6C 122.9(10) 1_555 1_555 1_555 no C5C C6C C7C 120.5(10) 1_555 1_555 1_555 no C6C C7C C8C 124.7(10) 1_555 1_555 1_555 no C6C C7C C11C 118.2(10) 1_555 1_555 1_555 no C8C C7C C11C 117.1(10) 1_555 1_555 1_555 no C7C C8C C9C 119.4(10) 1_555 1_555 1_555 no C8C C9C C10C 120.6(10) 1_555 1_555 1_555 no N2C C10C C9C 121.8(9) 1_555 1_555 1_555 no N2C C11C C7C 124.0(9) 1_555 1_555 1_555 no N2C C11C C12C 114.8(9) 1_555 1_555 1_555 no C7C C11C C12C 121.2(9) 1_555 1_555 1_555 no N1C C12C C4C 123.7(9) 1_555 1_555 1_555 no N1C C12C C11C 116.5(9) 1_555 1_555 1_555 no C4C C12C C11C 119.9(9) 1_555 1_555 1_555 no I1 Hg I2 107.88(3) 1_555 1_555 1_555 no I1 Hg I3 106.18(3) 1_555 1_555 1_555 no I1 Hg I4 110.57(3) 1_555 1_555 1_555 no I2 Hg I3 113.72(3) 1_555 1_555 1_555 no I2 Hg I4 106.03(3) 1_555 1_555 1_555 no I3 Hg I4 112.42(3) 1_555 1_555 1_555 no C1D1 N1D1 C2D1 126.5(7) 1_555 1_555 1_555 no C1D1 N1D1 C3D1 117.1(9) 1_555 1_555 1_555 no C2D1 N1D1 C3D1 116.4(9) 1_555 1_555 1_555 no O1D1 C1D1 N1D1 122.0(7) 1_555 1_555 1_555 no data_DID294_A-(dmso)(H2O) _database_code_CSD 212716 _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C36 H24 Fe N6 2+,Hg I4 2-,C2 H6 O S,H2 O' _chemical_formula_sum 'C38 H32 Fe Hg I4 N6 O2 S' _chemical_formula_iupac ? _chemical_formula_weight 1400.8 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.442(11) _cell_length_b 12.816(7) _cell_length_c 14.937(9) _cell_angle_alpha 82.22(4) _cell_angle_beta 81.78(4) _cell_angle_gamma 82.97(4) _cell_volume 2136(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.18 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304.0 _exptl_absorpt_coefficient_mu 6.875 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.22 _exptl_absorpt_correction_T_max 0.53 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 6139 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_theta_max 23 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 5869 _reflns_number_gt 3960 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.071 _refine_ls_wR_factor_ref 0.088 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3960 _refine_ls_number_parameters 260 _refine_ls_goodness_of_fit_ref 1.67 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.005 _refine_diff_density_max 3.96 _refine_diff_density_min -2.44 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Fe 0.3885(2) 0.2288(2) 0.2131(2) 0.0430(6) Uani Fe 1.0 N1A 0.5057(13) 0.2760(10) 0.1082(9) 0.049(3) Uani N 1.0 N2A 0.5281(13) 0.1339(11) 0.2519(10) 0.051(3) Uani N 1.0 C1A 0.4904(18) 0.3420(14) 0.0328(12) 0.059(3) Uani C 1.0 C2A 0.5803(21) 0.3665(16) -0.0339(14) 0.072(4) Uani C 1.0 C3A 0.6934(20) 0.3225(17) -0.0234(14) 0.074(4) Uani C 1.0 C4A 0.7190(18) 0.2512(17) 0.0527(14) 0.066(3) Uani C 1.0 C5A 0.8288(18) 0.1966(19) 0.0742(17) 0.078(5) Uani C 1.0 C6A 0.8410(18) 0.1208(20) 0.1467(17) 0.083(6) Uani C 1.0 C7A 0.7426(18) 0.0986(17) 0.2084(15) 0.072(4) Uani C 1.0 C8A 0.7451(21) 0.0180(19) 0.2814(17) 0.086(6) Uani C 1.0 C9A 0.6435(21) 0.0014(17) 0.3363(16) 0.082(5) Uani C 1.0 C10A 0.5323(18) 0.0592(14) 0.3191(13) 0.063(3) Uani C 1.0 C11A 0.6330(16) 0.1530(14) 0.1930(13) 0.056(3) Uani C 1.0 C12A 0.6172(16) 0.2306(14) 0.1174(12) 0.053(3) Uani C 1.0 N1B 0.2850(12) 0.1656(10) 0.3192(9) 0.045(2) Uani N 1.0 N2B 0.3390(12) 0.1168(10) 0.1515(10) 0.047(2) Uani N 1.0 C1B 0.2634(15) 0.1888(13) 0.4044(12) 0.052(2) Uani C 1.0 C2B 0.1993(17) 0.1281(15) 0.4742(13) 0.062(3) Uani C 1.0 C3B 0.1491(17) 0.0413(15) 0.4543(14) 0.067(2) Uani C 1.0 C4B 0.1659(16) 0.0192(14) 0.3643(14) 0.061(2) Uani C 1.0 C5B 0.1158(18) -0.0673(15) 0.3343(17) 0.074(2) Uani C 1.0 C6B 0.1354(19) -0.0832(15) 0.2457(18) 0.076(2) Uani C 1.0 C7B 0.2098(17) -0.0242(14) 0.1782(15) 0.065(2) Uani C 1.0 C8B 0.2336(20) -0.0403(15) 0.0848(16) 0.074(3) Uani C 1.0 C9B 0.3123(19) 0.0199(15) 0.0326(14) 0.068(3) Uani C 1.0 C10B 0.3623(16) 0.0998(13) 0.0657(13) 0.054(2) Uani C 1.0 C11B 0.2610(15) 0.0596(13) 0.2070(13) 0.051(2) Uani C 1.0 C12B 0.2347(15) 0.0799(13) 0.2996(13) 0.050(2) Uani C 1.0 N1C 0.2516(12) 0.3305(10) 0.1774(10) 0.047(2) Uani N 1.0 N2C 0.4176(12) 0.3458(10) 0.2792(9) 0.047(3) Uani N 1.0 C1C 0.1711(16) 0.3259(14) 0.1232(13) 0.054(3) Uani C 1.0 C2C 0.0786(17) 0.4024(15) 0.1084(14) 0.065(4) Uani C 1.0 C3C 0.0677(17) 0.4908(15) 0.1519(15) 0.067(4) Uani C 1.0 C4C 0.1509(17) 0.5006(14) 0.2072(14) 0.059(3) Uani C 1.0 C5C 0.1496(18) 0.5928(14) 0.2600(15) 0.066(3) Uani C 1.0 C6C 0.2344(18) 0.6017(14) 0.3063(15) 0.066(3) Uani C 1.0 C7C 0.3325(17) 0.5205(14) 0.3167(13) 0.059(2) Uani C 1.0 C8C 0.4244(18) 0.5237(15) 0.3652(14) 0.065(3) Uani C 1.0 C9C 0.5115(18) 0.4413(15) 0.3731(14) 0.064(3) Uani C 1.0 C10C 0.5045(16) 0.3519(13) 0.3286(13) 0.054(3) Uani C 1.0 C11C 0.3341(15) 0.4291(13) 0.2730(12) 0.050(2) Uani C 1.0 C12C 0.2439(15) 0.4203(13) 0.2208(12) 0.050(2) Uani C 1.0 Hg 0.28965(7) 0.30570(6) 0.78527(6) 0.0584(3) Uani Hg 1.0 I1 0.1014(1) 0.1971(1) 0.8819(1) 0.0716(5) Uani I 1.0 I2 0.2812(1) 0.4900(1) 0.8640(1) 0.0720(5) Uani I 1.0 I3 0.5030(1) 0.1832(1) 0.7969(1) 0.0802(5) Uani I 1.0 I4 0.2445(2) 0.3558(1) 0.6040(1) 0.0923(6) Uani I 1.0 S1D 0.9598(9) 0.2682(8) 0.3850(9) 0.101(8) Uani S 0.60 O1D 0.8986(30) 0.1929(28) 0.4485(29) 0.195(9) Uani O 0.60 C1D 0.8466(34) 0.3379(31) 0.3186(31) 0.128(9) Uani C 0.60 C2D 0.9645(64) 0.3782(38) 0.4491(37) 0.184(9) Uani C 0.60 S1D' 0.8444(19) 0.3073(18) 0.4255(17) 0.148(8) Uani S 0.40 O1D' 0.8428(59) 0.2053(33) 0.4781(36) 0.258(9) Uani O 0.40 C1D' 0.9758(64) 0.3582(67) 0.4512(52) 0.179(8) Uani C 0.40 C2D' 0.9108(60) 0.2797(54) 0.3120(29) 0.131(9) Uani C 0.40 OW1 0.6181(30) 0.2084(29) 0.5057(17) 0.245(9) Uani O 0.60 OW1' 0.6285(47) 0.1774(46) 0.5438(26) 0.245(9) Uani O 0.40 HC1A 0.4083 0.3754 0.0249 0.063 Uani H 1.0 HC2A 0.5640 0.4158 -0.0896 0.087 Uani H 1.0 HC3A 0.7598 0.3418 -0.0717 0.089 Uani H 1.0 HC5A 0.9024 0.2150 0.0334 0.092 Uani H 1.0 HC6A 0.9205 0.0816 0.1552 0.100 Uani H 1.0 HC8A 0.8210 -0.0264 0.2927 0.106 Uani H 1.0 HC9A 0.6458 -0.0531 0.3909 0.099 Uani H 1.0 HC10A 0.4578 0.0418 0.3591 0.065 Uani H 1.0 HC1B 0.2948 0.2531 0.4190 0.054 Uani H 1.0 HC2B 0.1893 0.1464 0.5381 0.071 Uani H 1.0 HC3B 0.1024 -0.0036 0.5032 0.079 Uani H 1.0 HC5B 0.0669 -0.1148 0.3793 0.086 Uani H 1.0 HC6B 0.0952 -0.1400 0.2265 0.091 Uani H 1.0 HC8B 0.1944 -0.0932 0.0592 0.090 Uani H 1.0 HC9B 0.3361 0.0072 -0.0324 0.078 Uani H 1.0 HC10B 0.4168 0.1445 0.0229 0.054 Uani H 1.0 HC1C 0.1781 0.2618 0.0906 0.056 Uani H 1.0 HC2C 0.0205 0.3935 0.0666 0.075 Uani H 1.0 HC3C 0.0004 0.5474 0.1436 0.077 Uani H 1.0 HC5C 0.0809 0.6491 0.2593 0.076 Uani H 1.0 HC6C 0.2320 0.6674 0.3361 0.075 Uani H 1.0 HC8C 0.4280 0.5879 0.3957 0.076 Uani H 1.0 HC9C 0.5781 0.4440 0.4091 0.074 Uani H 1.0 HC10C 0.5673 0.2907 0.3345 0.056 Uani H 1.0 H1C1D 0.8276 0.2910 0.2756 0.220 Uani H 0.60 H2C1D 0.7733 0.3578 0.3605 0.176 Uani H 0.60 H3C1D 0.8766 0.4035 0.2833 0.153 Uani H 0.60 H1C2D 1.0240 0.3580 0.4930 0.300 Uani H 0.60 H2C2D 0.9876 0.4413 0.4062 0.175 Uani H 0.60 H3C2D 0.8843 0.3957 0.4834 0.281 Uani H 0.60 H1C1D' 0.9605 0.3800 0.5139 0.352 Uani H 0.40 H2C1D' 1.0443 0.3017 0.4477 0.194 Uani H 0.40 H3C1D' 0.9949 0.4208 0.4060 0.159 Uani H 0.40 H1C2D' 0.8523 0.2492 0.2820 0.226 Uani H 0.40 H2C2D' 0.9337 0.3468 0.2750 0.154 Uani H 0.40 H3C2D' 0.9831 0.2278 0.3166 0.173 Uani H 0.40 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Fe 0.049(1) 0.031(1) 0.050(2) -0.006(1) -0.010(1) -0.007(1) Fe N1A 0.063(3) 0.040(4) 0.047(4) -0.013(3) -0.002(3) -0.017(3) N N2A 0.062(3) 0.041(4) 0.054(4) -0.001(3) -0.012(3) -0.016(3) N C1A 0.082(4) 0.048(4) 0.048(4) -0.018(4) -0.002(3) -0.011(3) C C2A 0.101(6) 0.065(7) 0.053(5) -0.033(5) 0.008(5) -0.014(4) C C3A 0.089(5) 0.077(8) 0.063(5) -0.040(5) 0.017(5) -0.033(4) C C4A 0.066(3) 0.072(6) 0.068(5) -0.026(3) 0.009(4) -0.041(4) C C5A 0.060(4) 0.097(9) 0.091(8) -0.020(3) 0.007(4) -0.062(6) C C6A 0.057(4) 0.099(9) 0.103(9) 0.001(3) -0.010(3) -0.061(6) C C7A 0.061(4) 0.075(6) 0.086(6) 0.008(4) -0.018(3) -0.040(4) C C8A 0.081(4) 0.081(7) 0.100(8) 0.024(5) -0.033(5) -0.031(5) C C9A 0.094(5) 0.066(6) 0.085(7) 0.020(5) -0.032(5) -0.013(4) C C10A 0.080(4) 0.047(4) 0.062(5) 0.004(4) -0.019(3) -0.010(3) C C11A 0.057(4) 0.052(4) 0.063(4) -0.002(3) -0.010(3) -0.027(3) C C12A 0.059(4) 0.051(4) 0.056(4) -0.014(3) -0.001(3) -0.027(3) C N1B 0.047(4) 0.035(3) 0.053(4) 0.000(3) -0.009(3) -0.007(3) N N2B 0.054(4) 0.033(3) 0.057(4) -0.002(3) -0.017(3) -0.013(3) N C1B 0.056(4) 0.044(4) 0.052(4) 0.006(3) -0.006(3) -0.006(3) C C2B 0.062(6) 0.056(6) 0.059(4) 0.009(4) 0.000(4) 0.003(3) C C3B 0.057(5) 0.056(6) 0.077(4) 0.002(4) 0.001(5) 0.012(4) C C4B 0.052(4) 0.045(4) 0.083(4) -0.007(3) -0.009(4) 0.006(4) C C5B 0.061(5) 0.047(4) 0.113(7) -0.016(4) -0.019(5) 0.010(5) C C6B 0.072(6) 0.044(4) 0.119(8) -0.020(4) -0.033(6) -0.002(5) C C7B 0.071(5) 0.039(3) 0.094(5) -0.013(3) -0.032(4) -0.012(4) C C8B 0.094(8) 0.045(5) 0.099(6) -0.010(4) -0.044(6) -0.023(5) C C9B 0.092(8) 0.046(5) 0.076(4) 0.000(4) -0.036(5) -0.026(5) C C10B 0.069(5) 0.039(3) 0.059(4) 0.001(3) -0.022(3) -0.018(3) C C11B 0.055(4) 0.034(3) 0.069(4) -0.007(3) -0.020(3) -0.010(3) C C12B 0.049(4) 0.036(3) 0.066(4) -0.005(3) -0.012(3) -0.003(3) C N1C 0.048(4) 0.037(3) 0.058(5) -0.010(3) -0.012(3) -0.002(3) N N2C 0.052(4) 0.037(3) 0.056(5) -0.013(3) -0.011(3) -0.004(3) N C1C 0.053(4) 0.045(3) 0.069(5) -0.009(3) -0.019(4) -0.002(3) C C2C 0.058(5) 0.052(4) 0.086(8) -0.004(4) -0.026(5) -0.001(5) C C3C 0.059(5) 0.049(4) 0.091(9) 0.000(4) -0.020(4) -0.001(4) C C4C 0.057(4) 0.041(3) 0.078(6) -0.003(3) -0.011(3) -0.003(3) C C5C 0.069(6) 0.041(3) 0.087(8) -0.001(4) -0.006(5) -0.008(4) C C6C 0.077(7) 0.040(3) 0.082(8) -0.007(3) -0.005(5) -0.013(4) C C7C 0.070(5) 0.039(3) 0.069(5) -0.012(3) -0.009(4) -0.011(3) C C8C 0.082(7) 0.046(4) 0.075(7) -0.017(4) -0.016(5) -0.016(5) C C9C 0.077(6) 0.050(4) 0.075(7) -0.019(4) -0.023(5) -0.014(5) C C10C 0.060(4) 0.044(3) 0.064(5) -0.015(3) -0.018(3) -0.007(3) C C11C 0.056(3) 0.036(3) 0.060(4) -0.011(2) -0.008(3) -0.005(3) C C12C 0.052(4) 0.037(3) 0.062(4) -0.008(3) -0.009(3) -0.003(3) C Hg 0.0589(5) 0.0498(5) 0.0703(6) -0.0054(4) -0.0115(4) -0.0173(4) Hg I1 0.0554(8) 0.0592(8) 0.100(1) -0.0099(6) -0.0050(7) -0.0088(8) I I2 0.091(1) 0.0518(8) 0.081(1) -0.0133(7) -0.0156(8) -0.0258(7) I I3 0.0650(9) 0.0677(9) 0.111(1) 0.0093(7) -0.0231(8) -0.0248(9) I I4 0.130(2) 0.083(1) 0.074(1) -0.009(1) -0.037(1) -0.0209(8) I S1D 0.076(9) 0.060(8) 0.164(9) -0.002(5) -0.036(7) 0.016(6) S O1D 0.139(9) 0.139(9) 0.289(9) -0.051(9) -0.078(9) 0.122(9) O C1D 0.118(9) 0.072(9) 0.201(9) -0.014(7) -0.082(9) 0.025(9) C C2D 0.253(9) 0.155(9) 0.166(9) -0.021(9) -0.083(9) -0.038(9) C S1D' 0.109(9) 0.131(9) 0.179(9) -0.008(7) 0.026(9) 0.026(9) S O1D' 0.193(9) 0.241(9) 0.294(9) -0.073(9) -0.013(9) 0.160(9) O C1D' 0.247(9) 0.152(9) 0.160(9) -0.029(9) -0.093(9) -0.015(9) C C2D' 0.149(9) 0.091(9) 0.164(9) -0.002(8) -0.054(9) -0.025(9) C OW1 0.337(9) 0.305(9) 0.074(9) 0.222(9) -0.145(9) -0.054(9) O OW1' 0.337(9) 0.305(9) 0.074(9) 0.222(9) -0.145(9) -0.054(9) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1A 1.991(14) 1_555 1_555 no Fe N2A 1.991(13) 1_555 1_555 no Fe N1B 1.980(14) 1_555 1_555 no Fe N2B 1.983(13) 1_555 1_555 no Fe N1C 1.996(13) 1_555 1_555 no Fe N2C 1.988(14) 1_555 1_555 no N1A C1A 1.332(21) 1_555 1_555 no N1A C12A 1.353(21) 1_555 1_555 no N2A C10A 1.291(22) 1_555 1_555 no N2A C11A 1.409(22) 1_555 1_555 no C1A C2A 1.361(26) 1_555 1_555 no C2A C3A 1.368(30) 1_555 1_555 no C3A C4A 1.401(30) 1_555 1_555 no C4A C5A 1.418(29) 1_555 1_555 no C4A C12A 1.429(25) 1_555 1_555 no C5A C6A 1.365(33) 1_555 1_555 no C6A C7A 1.381(30) 1_555 1_555 no C7A C8A 1.399(31) 1_555 1_555 no C7A C11A 1.391(25) 1_555 1_555 no C8A C9A 1.345(32) 1_555 1_555 no C9A C10A 1.430(27) 1_555 1_555 no C11A C12A 1.417(26) 1_555 1_555 no N1B C1B 1.327(20) 1_555 1_555 no N1B C12B 1.384(21) 1_555 1_555 no N2B C10B 1.314(21) 1_555 1_555 no N2B C11B 1.343(21) 1_555 1_555 no C1B C2B 1.390(25) 1_555 1_555 no C2B C3B 1.397(28) 1_555 1_555 no C3B C4B 1.394(27) 1_555 1_555 no C4B C5B 1.456(28) 1_555 1_555 no C4B C12B 1.374(25) 1_555 1_555 no C5B C6B 1.349(30) 1_555 1_555 no C6B C7B 1.421(29) 1_555 1_555 no C7B C8B 1.421(29) 1_555 1_555 no C7B C11B 1.427(24) 1_555 1_555 no C8B C9B 1.349(29) 1_555 1_555 no C9B C10B 1.407(25) 1_555 1_555 no C11B C12B 1.424(24) 1_555 1_555 no N1C C1C 1.321(21) 1_555 1_555 no N1C C12C 1.384(21) 1_555 1_555 no N2C C10C 1.336(21) 1_555 1_555 no N2C C11C 1.345(20) 1_555 1_555 no C1C C2C 1.373(23) 1_555 1_555 no C2C C3C 1.365(27) 1_555 1_555 no C3C C4C 1.374(26) 1_555 1_555 no C4C C5C 1.505(27) 1_555 1_555 no C4C C12C 1.403(23) 1_555 1_555 no C5C C6C 1.294(27) 1_555 1_555 no C6C C7C 1.444(25) 1_555 1_555 no C7C C8C 1.369(26) 1_555 1_555 no C7C C11C 1.413(24) 1_555 1_555 no C8C C9C 1.365(26) 1_555 1_555 no C9C C10C 1.415(24) 1_555 1_555 no C11C C12C 1.403(24) 1_555 1_555 no Hg I1 2.821(2) 1_555 1_555 no Hg I2 2.764(1) 1_555 1_555 no Hg I3 2.751(1) 1_555 1_555 no Hg I4 2.804(2) 1_555 1_555 no S1D O1D 1.432(24) 1_555 1_555 no S1D C1D 1.818(25) 1_555 1_555 no S1D C2D 1.818(25) 1_555 1_555 no S1D' O1D' 1.432(24) 1_555 1_555 no S1D' C1D' 1.818(25) 1_555 1_555 no S1D' C2D' 1.818(25) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Fe N2A 83.1(6) 1_555 1_555 1_555 no N1A Fe N1B 173.0(5) 1_555 1_555 1_555 no N1A Fe N2B 94.1(6) 1_555 1_555 1_555 no N1A Fe N1C 96.5(6) 1_555 1_555 1_555 no N1A Fe N2C 90.7(6) 1_555 1_555 1_555 no N2A Fe N1B 90.4(6) 1_555 1_555 1_555 no N2A Fe N2B 91.5(5) 1_555 1_555 1_555 no N2A Fe N1C 176.7(6) 1_555 1_555 1_555 no N2A Fe N2C 93.8(5) 1_555 1_555 1_555 no N1B Fe N2B 83.3(6) 1_555 1_555 1_555 no N1B Fe N1C 90.1(5) 1_555 1_555 1_555 no N1B Fe N2C 92.5(6) 1_555 1_555 1_555 no N2B Fe N1C 91.7(5) 1_555 1_555 1_555 no N2B Fe N2C 173.2(6) 1_555 1_555 1_555 no N1C Fe N2C 82.9(6) 1_555 1_555 1_555 no Fe N1A C1A 130.4(13) 1_555 1_555 1_555 no Fe N1A C12A 112.2(12) 1_555 1_555 1_555 no C1A N1A C12A 117.4(16) 1_555 1_555 1_555 no Fe N2A C10A 129.1(14) 1_555 1_555 1_555 no Fe N2A C11A 111.8(11) 1_555 1_555 1_555 no C10A N2A C11A 119.1(16) 1_555 1_555 1_555 no N1A C1A C2A 123.6(19) 1_555 1_555 1_555 no C1A C2A C3A 118.8(20) 1_555 1_555 1_555 no C2A C3A C4A 122.1(19) 1_555 1_555 1_555 no C3A C4A C5A 130.0(20) 1_555 1_555 1_555 no C3A C4A C12A 113.9(19) 1_555 1_555 1_555 no C5A C4A C12A 116.1(20) 1_555 1_555 1_555 no C4A C5A C6A 124.6(20) 1_555 1_555 1_555 no C5A C6A C7A 119.4(20) 1_555 1_555 1_555 no C6A C7A C8A 123.4(21) 1_555 1_555 1_555 no C6A C7A C11A 118.6(22) 1_555 1_555 1_555 no C8A C7A C11A 117.8(21) 1_555 1_555 1_555 no C7A C8A C9A 118.7(20) 1_555 1_555 1_555 no C8A C9A C10A 122.1(21) 1_555 1_555 1_555 no N2A C10A C9A 120.1(19) 1_555 1_555 1_555 no N2A C11A C7A 122.1(18) 1_555 1_555 1_555 no N2A C11A C12A 114.7(16) 1_555 1_555 1_555 no C7A C11A C12A 123.3(19) 1_555 1_555 1_555 no N1A C12A C4A 124.1(18) 1_555 1_555 1_555 no N1A C12A C11A 117.9(16) 1_555 1_555 1_555 no C4A C12A C11A 117.9(18) 1_555 1_555 1_555 no Fe N1B C1B 130.4(12) 1_555 1_555 1_555 no Fe N1B C12B 112.2(11) 1_555 1_555 1_555 no C1B N1B C12B 117.2(15) 1_555 1_555 1_555 no Fe N2B C10B 129.4(13) 1_555 1_555 1_555 no Fe N2B C11B 111.7(11) 1_555 1_555 1_555 no C10B N2B C11B 118.5(15) 1_555 1_555 1_555 no N1B C1B C2B 123.3(18) 1_555 1_555 1_555 no C1B C2B C3B 119.3(18) 1_555 1_555 1_555 no C2B C3B C4B 118.0(18) 1_555 1_555 1_555 no C3B C4B C5B 123.4(19) 1_555 1_555 1_555 no C3B C4B C12B 119.4(18) 1_555 1_555 1_555 no C5B C4B C12B 117.2(19) 1_555 1_555 1_555 no C4B C5B C6B 119.9(19) 1_555 1_555 1_555 no C5B C6B C7B 123.9(19) 1_555 1_555 1_555 no C6B C7B C8B 125.2(19) 1_555 1_555 1_555 no C6B C7B C11B 116.6(20) 1_555 1_555 1_555 no C8B C7B C11B 118.2(19) 1_555 1_555 1_555 no C7B C8B C9B 116.1(18) 1_555 1_555 1_555 no C8B C9B C10B 122.8(19) 1_555 1_555 1_555 no N2B C10B C9B 121.4(19) 1_555 1_555 1_555 no N2B C11B C7B 122.6(17) 1_555 1_555 1_555 no N2B C11B C12B 118.1(15) 1_555 1_555 1_555 no C7B C11B C12B 119.2(18) 1_555 1_555 1_555 no N1B C12B C4B 122.6(17) 1_555 1_555 1_555 no N1B C12B C11B 114.4(16) 1_555 1_555 1_555 no C4B C12B C11B 123.0(17) 1_555 1_555 1_555 no Fe N1C C1C 132.3(12) 1_555 1_555 1_555 no Fe N1C C12C 110.1(11) 1_555 1_555 1_555 no C1C N1C C12C 117.6(14) 1_555 1_555 1_555 no Fe N2C C10C 129.8(11) 1_555 1_555 1_555 no Fe N2C C11C 112.9(11) 1_555 1_555 1_555 no C10C N2C C11C 117.2(14) 1_555 1_555 1_555 no N1C C1C C2C 125.0(17) 1_555 1_555 1_555 no C1C C2C C3C 118.5(18) 1_555 1_555 1_555 no C2C C3C C4C 118.7(17) 1_555 1_555 1_555 no C3C C4C C5C 124.6(17) 1_555 1_555 1_555 no C3C C4C C12C 120.9(17) 1_555 1_555 1_555 no C5C C4C C12C 114.5(17) 1_555 1_555 1_555 no C4C C5C C6C 122.1(17) 1_555 1_555 1_555 no C5C C6C C7C 122.6(18) 1_555 1_555 1_555 no C6C C7C C8C 125.9(17) 1_555 1_555 1_555 no C6C C7C C11C 117.4(18) 1_555 1_555 1_555 no C8C C7C C11C 116.7(17) 1_555 1_555 1_555 no C7C C8C C9C 121.5(17) 1_555 1_555 1_555 no C8C C9C C10C 118.0(17) 1_555 1_555 1_555 no N2C C10C C9C 122.8(16) 1_555 1_555 1_555 no N2C C11C C7C 123.9(16) 1_555 1_555 1_555 no N2C C11C C12C 116.0(15) 1_555 1_555 1_555 no C7C C11C C12C 120.2(16) 1_555 1_555 1_555 no N1C C12C C4C 119.2(16) 1_555 1_555 1_555 no N1C C12C C11C 117.8(15) 1_555 1_555 1_555 no C4C C12C C11C 122.9(16) 1_555 1_555 1_555 no I1 Hg I2 105.85(5) 1_555 1_555 1_555 no I1 Hg I3 110.46(5) 1_555 1_555 1_555 no I1 Hg I4 107.71(6) 1_555 1_555 1_555 no I2 Hg I3 111.63(5) 1_555 1_555 1_555 no I2 Hg I4 109.53(5) 1_555 1_555 1_555 no I3 Hg I4 111.43(6) 1_555 1_555 1_555 no O1D S1D C1D 104.5(10) 1_555 1_555 1_555 no O1D S1D C2D 104.5(10) 1_555 1_555 1_555 no C1D S1D C2D 94.1(19) 1_555 1_555 1_555 no O1D' S1D' C1D' 104.5(10) 1_555 1_555 1_555 no O1D' S1D' C2D' 104.5(10) 1_555 1_555 1_555 no C1D' S1D' C2D' 94.1(19) 1_555 1_555 1_555 no